大豆中除草剂残留定性定量检测技术研究
|
摘要
本研究论文是国家“十五”食品安全重大专项课题“农兽药残留系统检测方法和快速筛选检测方法的建立”(2001BA804A11)和“农药残留检测技术研究”(2001BA804A17)课题研究的一部分。在充分调研和查新的基础上,课题针对除草剂残留检测技术的空白,在国内外残留限量(除草剂限量)规定的不断的严格和增加的情况下展开研究。
论文综述了18类已使用的除草剂的创制和应用历史、近年的发展趋势和推广情况,介绍了除草剂的理化性质和毒理学研究进展。综述了除草剂的最大残留限量的变化,特别是近年大幅度的变化情况,如日本的“肯定列表制度”所涉及的大豆用除草剂最大残留限量的情况,由于限量的变化和除草剂残留检测技术的缺乏而对我国大豆消费和进出口所产生的影响。据国内外大豆除草剂残留分析方法的现状,技术上的缺陷和依据现代仪器分析技术的进步所带来的分析方法技术指标的大幅度提高,系统研究了能够满足最大残留限量标准的除草剂残留的检测方法。
研究分别建立了二硝基苯胺类、苯氧羧酸类、磺酰脲类、三嗪类、酰胺类等多类常用除草剂残留检测方法,以适用于不同的检测目的。二硝基苯按类除草剂属于脂溶性化学物质,易溶于有机溶剂,另外分子中带有电负性原子,因此选择气相色谱/电子铺获检测器建立检测方法,方法灵敏度高、选择性好,同时建立了气相色谱/质谱确证检测参数。苯氧羧酸类除草剂由于是有机酸类除草剂,水溶性好,应用三氟化硼-乙醚/甲醇溶液衍生化的方式,使得苯氧羧酸类除草剂形成甲酯化产物,应用气相色谱/质谱建立了定性定量检测方法,方法的灵敏度达到了0.005 mg/kg。磺酰脲类除草剂在磷酸缓冲溶液/乙腈梯度洗脱下,完成分离和液相色谱定量检测。三嗪类除草剂经过方法学实验,以乙腈/水梯度洗脱,在228 nm波长下液相色谱/二极管矩阵检测器检测,各组分均获得良好的分离。根据酰胺类除草剂的性质,在优化提取分离条件下,以乙腈/水为流动相,在210nm波长下测定,获得很好的检测下限和分离度。
研究还建立了基于1.7μm小颗粒最新技术的超高效分析条件,UPLC~(TM)比传统HPLC具有更高的分离柱效。可以在很高的线速度、流速和反压下进行高效的分离工作,采用UPLC/MS/MS技术对14类除草剂共计111种在农业上广泛使用的除草剂进行了提取净化和分离条件实验研究,方法的最高灵敏度达到0.1mg/kg。
论文首次应用液相色谱/飞行时间质谱研究并建立了大豆中未知除草剂残留筛查检测方法。飞行时间质谱可以给出疑似除草剂残留的所检出化合物的精确分子量,据此完成未知靶标除草剂残留的筛查确证。该方法的建立解决了全未知样品的筛查检测技术关键,为国家植物源性农产品质量监控和抽查提供技术手段。
The study was based on the 10th five-year plan Food Safety Key Project "Establishment of systematic determination and rapid screening methods of pesticides and veterinary drugs residues"(2001BA804All) and "Study on pesticides residues determination technology" (2001BA804A17).The study was aimed at filling the blank of herbicides residues determination technology and meeting the international requirement of more and more stringent MRLs.
Our paper summarized the development and application history,trend in recent years and generalization of 18 kinds widely used pesticides.The physical and chemical properties and toxicological research were also introduced.This chapter also reviewed the change of pesticides MRLs values,especially the huge change in recent years.For example,the MRLs of the pesticides used in soybeans involved in Japan "positive list" were reviewed.The influence of the MRLs change and lack of determination technology on the soybean consumption and export was also analyzed.The chapter emphasized on the situation of analytical methods of pesticides residues in soybean in China and abroad.
In addition,the prohibited pesticides regulated in developed countries and some limitation standards on soybean in our country were also analyzed in the chapter.The toxicology and analytical methods of pesticides metabolites arisen recently in foreign countries were also reviewed.The establishment of systematic determination technology was put forward to meet the requirement of pesticides MRLs.
According to the pesticides classification,the determination methods of dinitroaniline, phenoxycarboxylic acids,sulfonyluerea,amides,triazines residues were demonstrated to meet the different requirements.Dinitroaniline herbicides were soluble in organic solvent and there were electronegative atoms in molecules,therefore,GC/ECD method which showed great sensitivity and selectivity was chosen and the parameters of GC-MS for confirmative determination was established.Phenoxycarboxylic acids herbicides belong to organic acid herbicides and were easily dissolved in water.To get the formate products,boron trifluoride-ether-methanol was used for derivation.Then the GC-MS method was established for both qualitative and quantitative analysis and the sensitivity of method was up to 0.005 mg/kg.The baseline separation and HPLC quantitative determination of sulfonyluerea herbicides were achieved using phosphate buffer/acetonitrile gradient elution and the method was reliable.In this part,the satisfactory detection limits and resolution were obtained under the optimal extraction conditions.Acetonitrile/ water were used as mobile phase and the wavelength was set at 210 nm.The mixture of triazine herbicides were well separated using HPLC/DAD method,the experimental conditions were acetonitrile/water gradient elution and 228 nm.
The ultra performance analytical method based on 1.7μm particles was established. Compared with HPLC,UPLC~(TM) has higher column efficiency and the separation could be achieved under higher flow rate and back pressure.UPLC/MS/MS method was used for the determination of 14 different kinds herbicides commonly used in agriculture,totally 111 compounds were extracted,purified and separated,the excellent results were obtained.The sensitivity of the method was up to 0.1 mg/kg.
HPLC-TOF-MS method was used for the screening and determination of unknown herbicides residues in soybean for the first time.TOF-MS could provide the accurate molecular weight for the suspicious herbicide residues,therefore,the screening and confirmation of the unknown targeted herbicide residues could be achieved.The establishment of the method solved the key problem of the screening technology of totally unknown samples and provided the technical support for the national farm produce residues monitoring and spot test.
论文综述了18类已使用的除草剂的创制和应用历史、近年的发展趋势和推广情况,介绍了除草剂的理化性质和毒理学研究进展。综述了除草剂的最大残留限量的变化,特别是近年大幅度的变化情况,如日本的“肯定列表制度”所涉及的大豆用除草剂最大残留限量的情况,由于限量的变化和除草剂残留检测技术的缺乏而对我国大豆消费和进出口所产生的影响。据国内外大豆除草剂残留分析方法的现状,技术上的缺陷和依据现代仪器分析技术的进步所带来的分析方法技术指标的大幅度提高,系统研究了能够满足最大残留限量标准的除草剂残留的检测方法。
研究分别建立了二硝基苯胺类、苯氧羧酸类、磺酰脲类、三嗪类、酰胺类等多类常用除草剂残留检测方法,以适用于不同的检测目的。二硝基苯按类除草剂属于脂溶性化学物质,易溶于有机溶剂,另外分子中带有电负性原子,因此选择气相色谱/电子铺获检测器建立检测方法,方法灵敏度高、选择性好,同时建立了气相色谱/质谱确证检测参数。苯氧羧酸类除草剂由于是有机酸类除草剂,水溶性好,应用三氟化硼-乙醚/甲醇溶液衍生化的方式,使得苯氧羧酸类除草剂形成甲酯化产物,应用气相色谱/质谱建立了定性定量检测方法,方法的灵敏度达到了0.005 mg/kg。磺酰脲类除草剂在磷酸缓冲溶液/乙腈梯度洗脱下,完成分离和液相色谱定量检测。三嗪类除草剂经过方法学实验,以乙腈/水梯度洗脱,在228 nm波长下液相色谱/二极管矩阵检测器检测,各组分均获得良好的分离。根据酰胺类除草剂的性质,在优化提取分离条件下,以乙腈/水为流动相,在210nm波长下测定,获得很好的检测下限和分离度。
研究还建立了基于1.7μm小颗粒最新技术的超高效分析条件,UPLC~(TM)比传统HPLC具有更高的分离柱效。可以在很高的线速度、流速和反压下进行高效的分离工作,采用UPLC/MS/MS技术对14类除草剂共计111种在农业上广泛使用的除草剂进行了提取净化和分离条件实验研究,方法的最高灵敏度达到0.1mg/kg。
论文首次应用液相色谱/飞行时间质谱研究并建立了大豆中未知除草剂残留筛查检测方法。飞行时间质谱可以给出疑似除草剂残留的所检出化合物的精确分子量,据此完成未知靶标除草剂残留的筛查确证。该方法的建立解决了全未知样品的筛查检测技术关键,为国家植物源性农产品质量监控和抽查提供技术手段。
The study was based on the 10th five-year plan Food Safety Key Project "Establishment of systematic determination and rapid screening methods of pesticides and veterinary drugs residues"(2001BA804All) and "Study on pesticides residues determination technology" (2001BA804A17).The study was aimed at filling the blank of herbicides residues determination technology and meeting the international requirement of more and more stringent MRLs.
Our paper summarized the development and application history,trend in recent years and generalization of 18 kinds widely used pesticides.The physical and chemical properties and toxicological research were also introduced.This chapter also reviewed the change of pesticides MRLs values,especially the huge change in recent years.For example,the MRLs of the pesticides used in soybeans involved in Japan "positive list" were reviewed.The influence of the MRLs change and lack of determination technology on the soybean consumption and export was also analyzed.The chapter emphasized on the situation of analytical methods of pesticides residues in soybean in China and abroad.
In addition,the prohibited pesticides regulated in developed countries and some limitation standards on soybean in our country were also analyzed in the chapter.The toxicology and analytical methods of pesticides metabolites arisen recently in foreign countries were also reviewed.The establishment of systematic determination technology was put forward to meet the requirement of pesticides MRLs.
According to the pesticides classification,the determination methods of dinitroaniline, phenoxycarboxylic acids,sulfonyluerea,amides,triazines residues were demonstrated to meet the different requirements.Dinitroaniline herbicides were soluble in organic solvent and there were electronegative atoms in molecules,therefore,GC/ECD method which showed great sensitivity and selectivity was chosen and the parameters of GC-MS for confirmative determination was established.Phenoxycarboxylic acids herbicides belong to organic acid herbicides and were easily dissolved in water.To get the formate products,boron trifluoride-ether-methanol was used for derivation.Then the GC-MS method was established for both qualitative and quantitative analysis and the sensitivity of method was up to 0.005 mg/kg.The baseline separation and HPLC quantitative determination of sulfonyluerea herbicides were achieved using phosphate buffer/acetonitrile gradient elution and the method was reliable.In this part,the satisfactory detection limits and resolution were obtained under the optimal extraction conditions.Acetonitrile/ water were used as mobile phase and the wavelength was set at 210 nm.The mixture of triazine herbicides were well separated using HPLC/DAD method,the experimental conditions were acetonitrile/water gradient elution and 228 nm.
The ultra performance analytical method based on 1.7μm particles was established. Compared with HPLC,UPLC~(TM) has higher column efficiency and the separation could be achieved under higher flow rate and back pressure.UPLC/MS/MS method was used for the determination of 14 different kinds herbicides commonly used in agriculture,totally 111 compounds were extracted,purified and separated,the excellent results were obtained.The sensitivity of the method was up to 0.1 mg/kg.
HPLC-TOF-MS method was used for the screening and determination of unknown herbicides residues in soybean for the first time.TOF-MS could provide the accurate molecular weight for the suspicious herbicide residues,therefore,the screening and confirmation of the unknown targeted herbicide residues could be achieved.The establishment of the method solved the key problem of the screening technology of totally unknown samples and provided the technical support for the national farm produce residues monitoring and spot test.
引文
[1]徐明文,王文萍.化学除草剂灭草应用效果调查[J].林业月报,1997,(9):17
[2]Acosta E J,Steefensen M B,Tichy et al.Removal of atrazine from water using covalent sequestration [J].J Agric Food Chem,2004,52:545-549
[3]刘伟,宫香余.黑龙江省大豆生产中药害现状及对策[J].大豆通报,2006,(2):37-39
[4]李贵,吴竞仑.大豆田化学除草剂的发展及其应用[J].江苏农业科学,2006,(6):198-202
[5]钟金传.中国大豆产业国际竞争力研究[博士论文].北京:中国农业大学,2005
[6]Arregui Mafia,Lenardon Argelia,Sanchez Daniel,Maitre L Maria.monitoring glyphosate residues in transgenic glyphosate-resist soybean[J].Pest Manag Sci 2003,(60) 163-166
[7]任卫东,杨云彭.化学除草剂发展近况[J].化学工程师,1997,(4):25-26
[8]李海屏.世界除草剂新品种开发进展及发展趋势[J].农资科技,2004,(2):29-35
[9]任康太,杨华铮.除草剂的现状及发展对策[J].江苏化工,2000,27(2):36-37
[10]Nandihalli U B,Duke M V,Ashmore J W,et al.Enantioselectivity of protoporphyrinogen oxidase-inhibiting herbicides[J].PesticSci,1994,40:265-277
[11]Omokawa H,Konnai M.Inhibition of Echinochloa crus-gallivar frumentacea seedling root elongation by chiral 1,3,5-triazinesin the dark[J].Pestic Sci,1992,35:83-86
[12]Omokawa H,Murata H,Kobayashi S.Chiral response of Oryzeaeand Paniceae plants in a ethyl-benzyl-3-p-tolyl urea agar medium[J].Pest Manag Sci,2004,60:59-64
[13]Omokawa H,Ryoo J H.Enantioselective response of rice and barnyard millet on root growth inhibition by optically active a-methylbenzyl phenylureas[J].Pestic Biochem Physiol,2001,70:1-6
[14]Omokawa H,Wu J,Hatzios K K.Mechanism of safening action of dymuron and its two onomethyl analogues bensulfuron-methyl injury to rice(Oryza sativa)[J].Pestic Biochem Physiol,1996,55:54-63
[15]Shimabukuro R H,Hoffer B L.Enantiomers of diclop-methyl and their role in herbicide mechanism of action[J].Pestic Biochem Physiol,1995,51:68-82
[16]William A.Opportunities for chiral agrochemicals[J].Pestic Sci,1996,46:3-9
[17]蒋木庚,王鸣华,杨春龙,等.新型旋光性农药的研究与展望[J].农药,2000,12:1-3
[18]Gerwick B C,Jackson L A,Handly J,et al.Preemergence and postemergence activities of the(R)and(S) enantiomers of haloxyfop[J].Weed Sci,1988,36:453-456
[19]苏少泉,滕春红,赵世君.最近15年世界转基因抗除草剂作物与除草剂品种的发展[J].农药研究与应用,2006,10(3):1-4
[20]苏少泉.生物除草剂的研究与开发[J].农药,2004,43(3):97-100
[21]中国农垦进出口公司.农田杂草化学防除大全[M].上海:上海科学技术文献出版社,1992:785
[22]胡笑形.2001年美国农药使用情况[J].农药科学与管理,2003,24(1):42-44
[23]Fae H.2003 Soybean weed control guide[J].Soybean Degist,2003,63(3):1-18
[24]张跃进,黄辉.我国农田化学除草历史回顾与发展对策[C],第六次全国杂草科学学术研讨会论 文集.桂林:广西民族出版社,1999:15-19
[25]张玉聚,孙化田,王春生.除草剂及其混用与农田杂草化学防治[M].北京:中国农业科技出版社,2000:159
[26]王险峰.进口农药应用手册[M].北京:中国农业出版社,2000
[27]黄春艳,陈铁保,王宇,等.28种除草剂对大豆的安全性及药害研究初报[J].植物保护,2003,29(1):31-34
[28]赵云和,张子丰,孙利.咪草烟土壤残留对后茬水稻的影响[J].农药,2006,45(3):189-190
[29]周顺启,于凤瑶,张代军,等.大豆不同耕作方法对化学除草效果的影响[J].大豆通报,2003,(6):7
[30]中华人民共和国农业部农药检定所.农药电子手册[EB].http://www.Chinapest-icide.gov.cn.2006-09-20.
[31]冯维卓.中国农田除草剂使用现状及存在问题[J].农药快讯,2001,(11):16-17
[32]刘伟,宫香余.黑龙江省大豆生产中药害现状及对策[J].大豆通报,2006,(2):37-39
[33]王焕民.对改善我国除草剂品种结构状况的思考[J].农药,2003,42(9):1-5
[34]卢向阳.几种大豆苗后除草剂与表面活性剂组合及其相互作用的研究[D].北京:中国农业大学,2001
[35]钟决龙.二苯醚类除草剂生产及大田应用现状[J].农药,2005,44(5):237-238
[36]刘长令,张运晓.国外部分农药品种在我国的知识产权保护状况[J].农药,2000,39(7):5-8
[37]王涛,贺红武,薛思佳.新颖除草剂研究进展[J].化学世界,2002,(11):608-614
[38]Alan J Tan,House William A,Parker Andrew,Canter E.Joy.transport and distribution of lindane and simazine in arivenine environment measurements in bed sediments and modeling[J].Pest Manag Sci 2004,(60)417-433
[39]匡华.大豆中苯氧羧酸除草剂的多残留检测技术研究[硕士论文].北京:中国农业大学,2006
[40]http://www.fsr.org.cn/2222.asp
[41]Gerald K Sims,Alison M Cupples.Factors controlling degradation of pesticides in soil[J].Pestic Sci,1999,(55):566-614
[42]Eiji Warabi,Kenji Usui,Yoshiyuki Tanaka,Hiroshi Matsumoto.resistance of a soybean cell line to oxyfluorfen by over production of nitochlordrial[J].Pest Manag Sci,2001,(57):743-748
[43]Liu D,Maguire R J,Lau Y.L,Pacepavicius G.J,Okamura H,Aoyama I.Factors Affecting Chemical Biodegradation,John Wiley & Sons,Inc.2000:476-438
[44]Gavrilescu M.Fate of pesticides in the environment and its bioremediation Eng.Life Sci,2005,(5):497-526
[45]Delinsky D.Amy,Bruckner V.James and Bartlett G.Michael.A review of analytical methods for the determination of trichloroethylene and its major metabolites chloral hydrate,trichloroacetic acid and dichloroacetic acid[J].Biomed.Chromatogr,2005,(19):617-639
[46]Sabine von Wiren-Lehr,Dieter Werner E.Komoa,Glagen,Heinrich Sandermann,JrIrene Scheunert.Mineralization of and its[~(14)C]Glyphosate Plant-Associated Residues in Arable Soils Originating from Different Farming Systems[J]. Pestic. Sci,1997,(51):436-442
[47] Rodrguez J, Mellado M., Corredor M. C., Pospil L, Hromadova M. Electrochemical. Reduction of Pyridinic Herbicides Picloram and Clopyralid on a Mercury Pool Electrode [J]. Electroanalysis, 2005,17(11):979-984
[48] Benedikt Gra β .Helmut Mayer, Jurgen Nolte, Gudrun Preu β , Ninette Zullei-Seibert. Studies on the metabolism of hydroxybenzonitrile herbicides:I. Mass spectrometric identification [J]. Pest Manag Sci,2000,(56):49-59
[49] Dayan E. Franck, Duke O.Stephen, Weete D.John Hancock H. Gary. Selectivity and Mode of Action of Carfentrazone-ethyl, a Novel Phenyl Triazolinone Herbicide [J]. Pestic. Sci, 1997,(51):65-73
[50] Dewez David, Marchand Mathieu, Eullaffroy Philippe, Popovic Radovan. Evaluation of the Effects of Diuron and Its Derivatives on Lemna gibba Using a Fluorescence Toxicity. Index Wiley Periodicals, Inc.2002 :493-501
[51] Avila A Liuis ,Massey H Joseph, Senseman A Scott, Armabrust L Kevin. Imazethapyr aqueous photolysis reaction quantum yield and hydroxyl radical rate constant [J]. J Agric Food Chem, 2006,(54):2635-2639
[52] Schneiderheinze J.M., Armstrong D.W., Berthod A. Plant and Soil Enantioselective Biodegradation of Racemic Phenoxyalkanoic Herbicides [J]. Chirality, 1999,(11 ):330-337
[53] Johnson Andrew.C, White Craig, Bhardwaj Clal, Dixon Andy, the ability of indigenous micro-organisms to degrade isoproputron atrazine and mecrop within aerobic UK aquifer system [J]. Pest Manag Sci,2003,(59): 1291-1302
[54] Babczinski Peter. Plant cell cultures as a model for the biochemistry of crop selectivity [J]. Pestic Sci, 1999,(55):633-675
[55] John PH Reade, Andrew H Cobb. Purification, characterization and comparison of glutathione S-transferases from black-grass (Alopecurus myosuroides Huds) biotypes [J]. Pestic Sci, 1999,(55):993-999
[56] Piutti Se'verine, Marchand Anne-Laure, Lagacherie Bernard, Fabrice Martin-Laurent and Guy Soulas. Effect of cropping cycles and repeated herbicide applications on the degradation of diclofopmethyl, bentazone, diuron, isoproturon and pendimethalin in soil [J]. Pest Manag Sci 2002,(58):303-312
[57] Pearson Robert, Godley Andrew, Carter Elise Investing the in situ degradation of atrazine in groundwater [J]. Pest Manag Sci 2006,(62):299-306
[58] Pirkko Laitinen, Katri Siimes, Liisa Eronen. Fate of the herbicides glyphosate glufosinate-ammonium, phenmedipham, ethofumesate and metamitron in two finnish arable soils [J]. Pest Manag Sci, 2006,(62):473-496
[59] Arregui Maria, Lenardon Argelia, Sanchez Daniel, Maitre L Maria, monitoring glyphosate residues in transgenic glyphosate-resist soybean [J]. Pest Manag Sci,2003,(60): 163-166
[60] 刘爱菊,朱鲁生,王军,孙瑞莲,林爱军．除草剂阿特拉津的环境毒理研究进展[J]．土壤与环境 2002,11(4):405-408
[61]Huang Sung-Ben,Thomas J Mayer,Yorkley A Robbert,Perez Rolando.Direct aqueous injection liquid chromatography/electropray ionization-mass spectrometry/mass spectrometry analysis of water for atrazine,simazine and their chlorotriazine metabolites[J].J.Agri Food Chem,2006,(40):122-125
[62]Quivet Etienne,Faure Rene,Geroges Joseph,Passe Jean-Qiiver.Photochemical degradation of imazamox in aqueous solution influence of metal ions and anionic species on the ultraviolet photolysis[J].J Agric Food Chem,2006,(54):3641-3645
[63]Kim Jim,Liu Kwang-Hueon,Kang Seung-Hun,Koo Suk-Jin.Degradation of the sulfonylurea herbicide LGC-42153 in flooded soil[J].Pest Manag Sci,2003,(59):1037-1042
[64]Patrizia Morrica,Paola Fidente and Serenella Seccia.Identification of photoproducts from imazosulfuron by HPLC[J].Biomed.Chromatogr,2004,(18):450-456
[65]苏少泉.除草剂的代谢与新品种创制[J].农药,2001,40:(9)1-3
[66]Jean Rouchoud,Marc Metsue,Michel Van Himme,Robent Bulke.Soil of metazuchlor in agronomic and vegetable crop fields[J].Weed Science,1992,(38):713-721
[67]苏少泉,滕春红,王春林.欧盟对农药的重新评定与我国除草剂品种发展[J].农药,2004,43(9):385-388
[68]Bowner,K H.Atrazine persistence and toxicity in two irrigated soils of Australia[J].Aus J Soil Res,1991,29:339-350
[69]Friesel P,Milde G,Stock R,et al.Impact of agricultural pesticide application on ground water in western Germany[A].In Proc 13th Congr.International Soil Sci,[C].Hamburg,1986:856-871
[70]Loch J P G,Van Dijk Looyard A,Zoetman B C.Organics in ground water[A].Proc.IAWPRC Conf [C].Guildford U K,1989,1:39-54
[71]Yassir A,Lagacherie B,Houots,et al.Microbial aspects of atrazine biodegradation in relation to history of soil treatment[J].Pestic Sci,1999,55:779-809
[72]Pick F E,Van Dyk L P,Botha E.Atrazine in ground and surface water in maize prod-uction areas of the transvaal[J].South Africa Chemosphere,1992,25:335-341
[73]Wehje G R,Spalding R F,Burnside O C,et al.Biological significance and fate of atra-zine under aquifer conditions[J].Weed Sci,1983,31:610-618
[74]Pensabene J W,Fiddler W,Donoghue D J.Supercritical fluid extraction of atrazine and other triazine herbicide from fortified and incurred eggs[J].J Agric Food Chem,2000,48:1668-1672
[75]杜柳涛,邬惠琼,杨杏芬,等.氟乐灵对大鼠肝、肾微粒体酶的影响[J].中国职业医学,2000,27(5):16-18
[76]Szekacs A,Trummer N,Adanyi N,et al.Developmentof a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[77]Heinrich Sandermann Jr.Bound and unextractable pesticidal plant residues chemical characterization and consumer exposure[J].Pest Manag Sci,2004,(60):613-623
[78]Michelangelo Anastassiades,Steven J.Lehotay.Fast and easy multiresidue method employing acetonitrile estraction/partitioning and dispersive solid-phase extraction for the Determination of Pesticide Residues in Peoduce[J].J AOAC Int,2003,(86):412-431
[79]Chu Xiao-Gang,Hu Xiao-Zhong,Yao Hui-Yuan.Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography-mass selective detection[J].J Chromatogra A,2005,(1063):201-210
[80]Vincze Adam,Yinon Jehuda.Tandem Mass Spectrometric Collision-induced Dissociation Study of in an Ion Trap s-Triazines Mass Spectrometer[J].J Mass Spectro,1997,(32):1320-1331
[81]Butz S.Heberer Th.,Stan H.J.Determination of phenoxyalkanoic acids and other acidic herbicides at the low ppt level in water applying solid-phase extraction with RP-C18 materi[J].J.Chromatogr.A,1994,(677):63-74
[82]匡华,储晓刚,侯玉霞.气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量[J].中国食品卫生杂志,2006,18(6):503-508
[83]霍江莲,李军,葛毅强,储晓刚.大豆中二硝基苯胺类除草剂多残留的气相色谱法定量检测及质谱确证[J].分析化学 2006,(34),特刊:S63-S67
[84]卫锋,董振霖,于玲.气相色谱—质谱联用法检测大米中多种苯氧羧酸除草剂[J].分析测试学报,2005,24(增刊):304-30
[85]张浩,刘伊玲,徐威.大豆中异丙甲草胺残留量分析方法研究[J].大豆科学,1998,17(1):88-90
[86]Serodio P.,Nogueira J.M.F.Multi-residue screening of endocrine disrupters chemicals in water samples by stir bar sorptive extraction-liquid resorption-capillary gas chromatography-mass spectrometry detection[J].Analytica Chimica Acta,2004,(517):21-32
[87]Toshihiro Fujii,Kazuhiro Hatanaka,Hiromi Arimoto,Yoshihiro Mitsutsuka.Surface Ionization Organic Mass Spectrometry of s-Triazine Herbicides[J].J Mass Spectr,1997,(32):408-412
[88]隋凯,李军,卫锋.固相萃取-高效液相色谱法同时检测大米中12种磺酰脲类除草剂的残留[J].色谱,2006,24(1):152-156
[89]祁彦,占春瑞,张新忠,杨强.高效液相色谱法测定大豆中13种三嗪类除草剂多残留量[J].分析化学,2006,(34):787-790
[90]祁彦,李淑娟,占春瑞,彭涛.高效液相色谱/质谱法测定大豆中磺酰脲类除草剂多残留量的研究[J].分析化学,2004,(32):1421-1425
[91]Schroder H F R.Mass spectrometric detection and identification of polar pesticides and their degradation products -a comparison of different ionzation method[J].J Environmental Monitoring and Assessment,1997,(44):503-513
[92]Clowers H.Brian,Steiner E.Wes,Dion M.Heather,Matz M.Laura,Tam Maggie,Tarver E.Edward,Hill H.Herbert Evaluation of Sulfonylurea Herbicides Using High Resolution Electrospray Ionization Ion Mobility Quadrupole Mass Spectrometry[J].Field Analytical Chemistry And Technology,2001,5(6):302-312
[93]Hidalgo C,Sancho J V,Hernandez F.Trace determination of triazine herbicides by means of coupled column liquid chromatography and large volume injection[J].Analytica Chimica Acta,1997,(338):223-229
[94]Giuseppe Ascenzo,Alessandra Gentili,Stefano Marchese.Optimization of High Performance Liquid Chromatography/Mass Spectrometry Apparatus for Determination of Imidazolinone Herbicides in Soil at Levels of a Few PPB[J].Rapid Commun.Mass Spectrom,1998,(12):1359-1365
[95]Carmen Molins,Elbert A.Hogendoorn,Ellen Dijkman,Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection[J].J Chromatogra A,2000,(869):487-496
[96]Renato Zanella,Ednei G.Prime,FabioF.Goncalves.Development and validation of a high-performance liquid chromatographic procedure for the determination of herbicide residues in surface and agriculture waters[J].J.Sep.Sci,2003,(26):935-938
[97]谢建军,朱亚红,朱嘉虹.除草剂双丙氨膦及代谢物草铵膦在土壤与桔子中的残留测定[J].农药,2003,42(8):18-20
[98]Satou Nemoto,Steven J.Lehotay.Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].J Agric.Food Chem,1998,(46):2190-2199
[99]许艇,邵晓龙,李季.除草剂2,4-D特异性多克隆抗体的制备及鉴定[J].生物技术2003,13(4):20
[100]施海燕,吴慧明,程敬丽等.2甲4氯人工抗原的合成与鉴定[J].农药学学报,2004,6(2):20-24
[101]Komarova NV,Kartsova LA.Optimizing Separation Conditions for Chlorophenoxycarboxylic Acid Herbicides in Natural and Potable Water Using Capillary Zone Electrophoresis[J].Anal Chem,2002,57(7):644-650
[102]Komarova NV,Kartsova LA.Determination of Herbicides of the Chlorophenoxycarboxylic Acid Type in Natural and Drinking Water by Capillary Zone Electrophoresis[J].Russian Journal of Applied Chemistry,2003,76(2):238-243
[103]Zhao Jing,Yi Guo-Xiang,He Su-Ping,Wang Bao-Min.Development of a monoclonal antibody -based enzyme-linked immunosorbent assay for the herbicide chlorimuron-ethyl[J].J Agric Food Chem,2006,(54):4948-4953
[104]Yazynina E.V.,Zherdev A.V.,Eremin S.A.,Popova V.A.,and Dzantiev B.B..Development of Enzyme Immunoassays for the Herbicide Chlorsulfuron[J].Applied Biochemistry and Microbiology,2002,38(1):9-14
[105]Dzantiev B.B,Yazynina E.V,Zherdev A.V.Determination of the herbicide chlorsulfuron by amperometric sensor based on separation-free bienzyme immunoassay[J].Sensors and Actuators B:Chemical,2004,98(2-3):254-261
[106]Yulaev M F,Sitdikov R A,Dmitrieva N M.development of a potentiometric immunosensorfor herbicide simazine and its application for food testing[J].Sensors and Actuators B,2001,(75):129-135
[107]Julia Yakovleva,Anatoly V.Zherdev,Valentina A.Popova,Sergei A.Eremin,Boris B.Dzantiev.Production of antibodies and development of enzyme-linked immunosorbent assays for the herbicide butachlor[J].Analytica Chimica Acta,2003,(491):1-13
[108]Francois MG Laurent,Rene Scalla.Metabolism and cell wall incorporation of phenoxyacetic acid in soybean cell suspension culture [J]. Pestic Sci,1999,(55):3-10
[109] http://www.cac.org.cn/
[110] E. Michael Thurman, Imma Ferrer. Amadeo Rodriguez Fern'andez-Alba[J]. J.Chromatogr A,2005, 1067:127-134
[111] E. Barcero-Barrachina, E. Moyano, M.T. Galceran [J]. J. Chromatogr A, 2004,1054:409-418
[1]Andras Szekacs,Nikoletta Trummer,Nora Adanyi et al.Development of a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[2]http://forum.globalimporter.net/view_topic/N11101105-26741-1.htm
[3]花日茂,汤锋,岳永德.甲基对硫磷、三唑酮和氟乐灵的同柱气相色谱分析[J].农药,1995,34(3):67-70
[4]黄灵芝,戴华,李拥军等.高效液相色谱法测定荞头中氟乐灵残留量[J].食品科学,2004,25(7):151-153
[5]赵凌菲,于春睿,赵国琴等.二甲戊乐灵的气相色谱分析[J].农药,1998,37(7):18-19
[6]祁彦,李淑娟,占春瑞等.高效液相色谱—质谱法测定大豆中磺酰脲类除草剂多残留量的研究[J].分析化学,2004,32:1436-1440
[7]Angel D'amato,Isabelia Semerabo,Carlo Bicchi.Simultaneous Determination of Linuron and Trifluralin Residues in Carrots and Their Pulp by Liquid Chromatography and Gas Chromatography[J].Journal of AOAC international,1993,76(3):657
[8]J.Engebretson,G.Hall,M.Hengel et al.Analysis of Pendimethalin Residues in Fruit,Nut,Vegetables,Grass,and Mint by Gas Chromatography[J].J.Agric.Food.Chem,2001,49:2198-2206
[9]Thomas A.Pressley,James E.Longbottom.The determination of dinitroaniline pesticides in industrial and municipal waste water.National technical information service,NO:PB82 156035
[10]Sheldon D.,West,Jack H.,Weston,Edgar W.,Day,JR.Gas Chromatographic Determination of Residue Level of the Herbicide Trifluralin,Benefin,Ethalfluralin,and Isopropalin in soil with Confirmation by Mass Selective Detection.[J].Assco.Of anal.Chem.1998,71(6):1082～1085
[11]Fuyu Guan,Kanako Watanabe,Akira Ishii et.Headspace solid-phase microextraction and gas chromatographic determination of dinitroaniline herbicides in human blood,urine and environmental water[J].Journal of Chromatography B,1998,714:205-213
[12]周培,陆贻通,伊雄海等.花生中氟乐灵农药残留的优化气相色谱测定法[J].上海交通大学学报,2003,21(3):205-207
[13]Julie Fillion,John Thorp.Multi-Pesticide Residue Analysis Utilizing SIM GC/MSD[J].HEWLETT PACKARD Gas-Phase Application Note,1995:228-348
[14]Akiko Tanable,Hideko Mitobe,Kuniki Kawaka et al.Monitoring of Herbicide in River water by gas chromatography-mass spectrometry and solid-phase extraction[J].Journal of chromatography A,1996,754:159-168
[15]Darcy D.Shackelford,Ron W.McCormick,Sheldon D.West et al.Determination of Ethalfluralin in Canola seed,Meal,and Refined Oil by Capillary Gas Chromatography with Mass Selective Detection[J].J.Agric.Food.Chem,2000,48:4422-4427
[16]Paolo Cabras,Marinella Melis.High-performance liquid chromatographic determination of dinitroaniline herbicides in soil and water[J].Journal of chromatography,1991,585:164-167
[17]Patrizia Vitali,Emanuela Venturini,Critina Bonora et al.Determination of triazines and dinitroanilines in waters by high-performance liquid chromatography after solid-phase extraction[J].journal of chromatography A,1994(660):219-222
[18]N.ruiz de erenchun,M.A.goicolea,Z.gomez de balugera et al.Determination of herbicide by reductive amperometric detection in liquid chromatography[J].Journal of chromatography A,1997,763:227-235
[19]Sibel Topuz,Gul Ozhan,Buket Alpertunga.Simultaneous determination of various pesticides in fruit juices by HPLC-DAD[J].Food Control,2005,16:87-92
[20]唐英章.现代食品安全检测技[M].北京:科学出版社,2004年9月
[21]Timothy M.,Fitzpatrick,Connie C.,Gehrig.Simultaneous Determination of Benefin and Trifluran in Pesticide Formulations by Gas Chromatography[J].J.ASSOC.OFF.ANAL.CHEM,1990,73(6):981-982
[22]张宇,范志先,许允成等.气质联用法测定二甲戊灵在马铃薯及土壤中的残留研究[J].吉林农业大学学报,2005,27(3):315-318
[23]朱鲁生,王军,谢慧等.二甲戊乐灵在土壤中的残留分析[J].农药.2004,43(11):512-514
[24]黄雅丽,毛黎娟,吴慧明等.二甲戊乐灵在甘蓝及土壤中的残留及消解动态研究[J].农业环境科学学报,2004,23(6):1147-1150
[25]Geoffrey B.Downer,Martin Hall,David N.B.Mallen.Determination of benefin and trifluralin residues by quantitative Gas-Liquid chromatography/Mass Spectrometry[J].J.Agric.Food Chem,1976,24(6):1223-1225
[26]Gyongyver Hegedus,Ivan Belai,Andras Szekacs.Development of an enzyme-linked Immunosorbent assay(ELISA) for the herbicide trifluralin[J].Analytica Chimica Acta,2000,421:121-133
[27]Seydou Traore,Jean-Jacques Aaron.Analysis of trifluralin and other dinitroaniline herbicide residues by zero-order and derivative ultraviolet spectrophometry[J].ANALYSIST,MAY 1989,VOL 114:609-613
[28]Andras Szekacs,Nikoletta Trummer,Nora Adanyi et al.Developmentof a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[29]Ludwig Huber,Validation of Analytical Methods:Review and Strategy,LC/GC International,July 2001
[1]刘长令主编.《世界农药大全-除草剂卷》[M].北京化学工业出版社,2002
[2]中国植物保护网http://www.ipmchina.net《21世纪除草剂发展展望》
[3]http://www.pmra-arla.gc.ca.2,4-Dichlorophenoxyacetic Acid Recent Developments
[4]Tibor Cserhati,Esther Forgacs.Phenoxyacetic acids:separation and quantitative determination[J].J Chromatogr.B,1998,717:157-178
[5]Joanna Davies,John Caseley.Herbicide safeners:a review[J].J Pestic Sci,1999,55:1043-1058
[6]http://www.bml.de/englisch/pflanzenschutz/risk3-1.htm Risk reduction in the field of plant protection products in Germany.Federal Ministry of Food,Agriculture and Forestry(FMFAF)(1998).
[7]出入境检验检疫行业标准SN0661-1997,粮谷中2,4,5-T的检测
[8]出入境检验检疫行业标准SN0687-1997,粮谷油籽中禾草灵的检测
[9]出入境检验检疫行业标准SN0195-1993,肉和肉制品中2,4-D的检测
[10]出入境检验检疫行业标准SN/T-1392-2004,肉和肉制品中MCPA,MCPB的检测
[11]http://www.fsr.org.cn食品安全限量、方法
[12]林维宣.各国食品中农药残留兽药残留限量规定(第三版)[M].大连,大连海事大学出版社,2002,28-209
[13]侯宇凯,侯松嵋等.拓宽气相色谱和高效液相色谱分析应用范围的有效途径—化学衍生法[J].化工标准·计量·质量,2001,5:29-31
[14]Moustapha Belmouden,Ali Assabbane,Yhia Ait Ichou.Adsorption characteristics of a phenoxy acetic acid herbicide on activated carbon[J].Environ Monit,2000,2:257-260
[15]S.Butze,Th.Heberer,H.-J.Stan Determination of phenoxyalkanoic acids and other acidic herbicides at the low ppt level in water applying solid-phase extraction with RP-C_(18) material[J].Chromatogr.A,1994,677:63-74
[16]USA EPA method 8041A Phenols By Gas Chromatography
[17]P.Cabras,C.Tuberoso,M.Melis,et al.Multiresidue method for pesticide determination in wine by high-performance liquid chromatography[J].J.Agric.Food Chem,.1992,40:817-819
[18]Balinova.Multiresidue determination of pesticides in plants by high-performance liquid chromatography following gel permeation chromatographic clean-up[J].J Chromatogr A,1998,823:11-16
[19]Aldo Lagana,Giovanna Fago,Alessondra Marinob.Liquid chromatography mass spectrometry tandem for multiresidue determination of selected post-emergence herbicides after soil column extraction[J].J Analytica Chimica Acta,2000,(415):41-56
[20]Paul R.Loconto.Isolation and recovery from water of selected chlorophenoxy acid herbicides and similar weak acid herbicides by solid-phase extraction HPLC and photodiode array detection[J].J liquid chromatogr,1991,14,7:1297-1314
[21]M.J.Incoruia.Mattina determination of chlorophenoxy acids using high performance liquid chromatography-particle beam mass spectrometry[J].J.Chromatogra,1991,542:385-395
[22]B.Rene,Geerdink,Paul G.M.Kieuhuis fast screening method for eight phenoxy acid herbicides-optimization procedures for flow-injection analysis-thermospray tandem mass spectrometry[J].J.Chromatogra,1993,647:329-339
[23]H.FR.Schroder.Mass spectrometric detection and identification of polar pesticides and their degradation products-a comparison of different ionzation method[J].Environmental Monitoring and Assessment,1997,44:503-513
[24]J.Patsias,E.Papadopoulou-Mourkidou.Rapid method for the ananlysis of a variety of chemical classes of pesticides insurface and ground waters by off-line solid-phase extraction and gas chromatography-ion trap mass spectrometry[J].J.Chromatogra,1996,740:83-98
[25]Karl-Heinz Bauer,Thomas P.Knepper,Anke Maes Analysis of polar organic micropollutants in water with ion chromatography-electrospray mass spectrometry[J].J.Chromatogr A,1999,837:117-128
[26]Tibor Cserhati,Esther Forgacs,Zdenek Deyl.Chromatographic determination of herbicide residues in various matrices[J].J.Biomed.Chromatogr,2004,18:350-359
[27]Stefano Marchese,Daniela Perret,Alessandra Gentili,et al.Determination of phenoxyacid herbicides and their phenolic metabolites in surface and drink water[J].Rapid Commun,Mass Spectrum,2002,16:134-141
[28]O.Pozo,E.Pitarch,J.V.Sancho,F.Hernandez.Determination of the herbicide 4-chloro-2-methylphenoxyacetic acid and its main metabolite,4-chloro-2-methylphenol in water and soil by liquid chromatography-electrospray tandem mass spectrometry[J].J.Chromatogr A,2001,923:75-85
[29]Su Tiana,Kozo Nakamurab,Tong Cuic,High-performance liquid chromatographic determinationof phenolic compounds in rice[J].J.Chromatogr A,2005(1063):121-128
[30]Adriana Farran,Santiago Ruiz.Application of solid-phase extraction and micellar electrokinetic capillary chromatography to the study of hydrolytic and photolytic degradation of phenoxy acid and phenylurea herbicides[J].J.Chromatogr.A,2004,1024:267-274
[31]N.V.Komarova,L.A.Kartsova.Optimizing Separation Conditions for Chlorophenoxycarboxylic Acid Herbicides in Natural and Potable Water Using Capillary Zone Electrophoresis[J].Anal Chem,2002,57(7):644-650
[32]N.V.Komarova,L.A.Kartsova.Determination of Herbicides of the Chlorophenoxycarboxylic Acid Type in Natural and Drinking Water by Capillary Zone Electrophoresis[J].Russian Journal of Applied Chemistry,2003,76(2):238-243
[33]Satou Nemoto,Steven J.Lehotay.Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].Agric.Food.Chem 1998,46:2190-2199
[34]蔡春平,王丹红,吴灵威等.苯氧羧酸类除草剂的毛细管电泳手性拆分研究[J].检验检疫科学,2004,14(6):23-25
[35]A.W.Garrison,P.Schmitt,A.Kettrup.Separation of phenoxy acid herbicides and their enantiomers by high-performance capillary electrophoresis[J].Chromatogr A,1994,684:317-327
[36]文岳中,蔡喜运,马云等.衍生化-手性毛细管色谱分离和测定水中的2,4-滴丙酸[J].分析化学32(11):1492-1494
[37]Gyrd-Hansen,N.and S.Dalgaard-Mikkelsen.The effect of phenoxy-herbicides on the hatchability of eggs and the viability of the chicks[J].Acta Pharmacol.Toxicol 1974,35:300-308
[38]许艇,邵晓龙,李季等.除草剂2,4-D特异性多克隆抗体的制备及鉴定[J].生物技术,2003,13(4):20-21
[39]施海燕,吴慧明,程敬丽等.2-甲-4-氯人工抗原的合成与鉴定[J].农药学学报,2004,6(2):20-24
[1]刘长令主编.世界农药大全-除草剂卷[M].北京,化学工业出版社,2002年
[2]海外传真.农药,2003,42(7):47
[3]林维宣.各国食品中农药残留兽药残留限量规定[M],大连,大连海事大学出版社,2002
[4]Prince J.L.,Guinivan R.A.Analysis of chlorimuron ethyl in crops by high performance liquid chromatography[J].J.Agric.Food Chem,1988,36:63-69
[5]Galletti G.C.,Bonetti A.High performance liquid chromatographic determination of sulfonylureas in soil and water[J].J.Chromtogr.A.,1995,692:27-37
[6]Menne J.H.,Janowitz K.Comparison of capillary electrophoresis and liquid chromatography for determination of sulfonylurea herbicides in soil[J].J.AOAC Internal.,1999,82(6):1534-1541
[7]Yumi A.,Naoki Y.and Masahiko T.Application of Multiresidue Screening Method to Pesticides for which Establishment of Maximum Residue Limits was Inquired in F.Y.1997[J].J.Food Hyg.Soc.Japan,2002,33:114-119
[8]Krynitsky J.A.Determination of sulfonylurea herbicides in grains by capillary electrophoresis[J].J.AOAC Int.,1997,80(2):392-340
[9]Nemoto S,Lehotay S.J.Analysis of multiple herbicides in soybeans using pres-surized liquid extraction and capillary elec-trophoresis[J].J.Agric.Food Chem,1998,46:2190-2199
[10]衣先众,姜得峰等.除草剂在大豆田应用研究[J].莱阳农学院学报,1999,16(1):25-27
[11]王晴 赵长山等.除草剂绿黄隆在小麦及大豆植株中残留分析方法的研究[J].化学工程师,1999,1:18-19
[12]默涛,张少军等.三氟羧草醚在大豆、茎叶及土壤中的残留分析方法研究[J].河北农业科学,1993,4:17-19
[1]刘长令.三嗪类除草剂的创制经纬[J].农药,2002,41(4):46
[2]孔志明,吴庆龙、黄健等.除草剂环嗪酮的毒性研究[J].农药,1994,33(5):31
[3]张一宾.世界三嗪类除草剂的发展概况.农药论坛
[4]朱忠林,单正军,蔡道基等.环嗪酮对生态环境影响评价研究.环境科学进展[J].1991,33(5):31
[5]王筱芬,刘毅,陶玉珍等.氰草津的毒理学研究[J].农药,1997,36(8):28-29
[6]潘洪吉,张群峰,李常平.苯嗪草酮原药的液相色谱分析方法[J].农药科学与管理,2000,21(2):4-5
[7]陈玲,郜洪文,董丽娴等.固相萃取—高效液相色谱法测定环境水样中的三嗪类化合物[J].色谱,2006,24(3):267-270
[8]任晋,黄翠玲,赵国栋等.固相萃取—高效液相色谱—质谱联机在线分析水中痕量除草剂[J].分析化学研究报告,2001,29(8):876-880
[9]刘长令.世界农药大全:除草剂卷[M].北京:化学工业出版社,2002
[10]苏少泉.酰胺类除草剂评述[J].农药,2002,41(11):1-5
[11]Institute for the Control of Agrochemicals,Ministry of Agriculture,P.R.China.Handbook of Practi cal Methods for the Determination of Pesticide Residues,Vol.1.Beijing:China Agriculture Publish ing House,1995
[12]黄宝华,叶秀薇.丙草胺的气相色谱分析[J].农药,1997,36(6):33-34
[1]Hidalgo C,Sancho J V,Hernandez F.Trace determination of triazine herbicides by means of coupled-column liquid chromatography and large volume injection[J].Analytica Chimica Acta,1997,338:223-229
[2]Giuseppe Ascenzo,Alessandra Gentili,Stefano Marchese.Determination of arylphenoxypropionic herbicides in water by liquid chromatography-electrospray mass spectrometry Rapid Commun[J].Mass Spectrom,1998,12,1359-1365
[3]Carmen Molins,Elbert A.Hogendoorn,Ellen Dijkman.Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection[J].J Chromatogra A,2000,869:487-496
[4]Renato Zanella,Ednei G.Prime,Fabio F.Goncalves,Determination of total arsenic by batch hydride generation atomic absorption spectrometry in injectable drugs containing high levels of Sb(V) as N-methylglucamine antimonate[J].J.Sep.Sci.,2003,26:.935-938
[5]Serodio P.,Nogueira J.M.F.Multi-residue screening of endocrine disrupters chemicals in water samples by stir bar sorptive extraction-liquid desorption-capillary gas chromatography-mass spectrometry detection[J].Analytica Chimica Acta,2004,517:21-32
[6]卫锋,董振霖,于玲等.气相色谱-质谱联用法检测大米中多种苯氧羧酸除草剂[J].分析测试学报,2005,24(增刊):304-306
[7]隋凯,李军,卫锋等.固相萃取-高效液相色谱法同时检测大米中12种磺酰脲类除草剂的残留[J].色谱,2006,24(1):152-156.
[8]张浩,刘伊玲,徐威等.大豆中异丙甲草胺残留量分析方法研究[J].大豆科学,1998,17(1):88-90.
[9]Satoru Nemoto,Steven J.Lehotay,Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].J.Agric.Food.Chem.,1998,46:2190-2199.
[1] http://www.cac.org.cn/
[2] B.A. Mamyrin. Time-of-flight mass spectrometry (concepts, achievements, and prospects) Int. [J]. Mass Spectrom, 2001,206:251-266
[3] E.M. Thurman, Imma Ferrer. Accurate mass analysis of ethanesulfonic acid degradates of acetochlor and alachlor using high-performance liquid chromatography and time-of-flight mass spectrometry [J]. J.Chromatogr A, 2002,957:3-9
[4] E. Michael Thurman, Imma Ferrer, Jerry A. Zweigenbaum. Discovering metabolites of post-harvest fungicides in citrus with liquid chromatography/time-of-flight mass spectrometry and ion trap tandem mass spectrometry [J]. J.Chromatogr A, 2005,1082: 71-80
[5] Emoto S, Steven JL. Agricultural pesticide residues in oysters and water from two Chesapeake bay tributaries[J]. J.Agric Food Chem, 1998,46: 2190-2199
[2]Acosta E J,Steefensen M B,Tichy et al.Removal of atrazine from water using covalent sequestration [J].J Agric Food Chem,2004,52:545-549
[3]刘伟,宫香余.黑龙江省大豆生产中药害现状及对策[J].大豆通报,2006,(2):37-39
[4]李贵,吴竞仑.大豆田化学除草剂的发展及其应用[J].江苏农业科学,2006,(6):198-202
[5]钟金传.中国大豆产业国际竞争力研究[博士论文].北京:中国农业大学,2005
[6]Arregui Mafia,Lenardon Argelia,Sanchez Daniel,Maitre L Maria.monitoring glyphosate residues in transgenic glyphosate-resist soybean[J].Pest Manag Sci 2003,(60) 163-166
[7]任卫东,杨云彭.化学除草剂发展近况[J].化学工程师,1997,(4):25-26
[8]李海屏.世界除草剂新品种开发进展及发展趋势[J].农资科技,2004,(2):29-35
[9]任康太,杨华铮.除草剂的现状及发展对策[J].江苏化工,2000,27(2):36-37
[10]Nandihalli U B,Duke M V,Ashmore J W,et al.Enantioselectivity of protoporphyrinogen oxidase-inhibiting herbicides[J].PesticSci,1994,40:265-277
[11]Omokawa H,Konnai M.Inhibition of Echinochloa crus-gallivar frumentacea seedling root elongation by chiral 1,3,5-triazinesin the dark[J].Pestic Sci,1992,35:83-86
[12]Omokawa H,Murata H,Kobayashi S.Chiral response of Oryzeaeand Paniceae plants in a ethyl-benzyl-3-p-tolyl urea agar medium[J].Pest Manag Sci,2004,60:59-64
[13]Omokawa H,Ryoo J H.Enantioselective response of rice and barnyard millet on root growth inhibition by optically active a-methylbenzyl phenylureas[J].Pestic Biochem Physiol,2001,70:1-6
[14]Omokawa H,Wu J,Hatzios K K.Mechanism of safening action of dymuron and its two onomethyl analogues bensulfuron-methyl injury to rice(Oryza sativa)[J].Pestic Biochem Physiol,1996,55:54-63
[15]Shimabukuro R H,Hoffer B L.Enantiomers of diclop-methyl and their role in herbicide mechanism of action[J].Pestic Biochem Physiol,1995,51:68-82
[16]William A.Opportunities for chiral agrochemicals[J].Pestic Sci,1996,46:3-9
[17]蒋木庚,王鸣华,杨春龙,等.新型旋光性农药的研究与展望[J].农药,2000,12:1-3
[18]Gerwick B C,Jackson L A,Handly J,et al.Preemergence and postemergence activities of the(R)and(S) enantiomers of haloxyfop[J].Weed Sci,1988,36:453-456
[19]苏少泉,滕春红,赵世君.最近15年世界转基因抗除草剂作物与除草剂品种的发展[J].农药研究与应用,2006,10(3):1-4
[20]苏少泉.生物除草剂的研究与开发[J].农药,2004,43(3):97-100
[21]中国农垦进出口公司.农田杂草化学防除大全[M].上海:上海科学技术文献出版社,1992:785
[22]胡笑形.2001年美国农药使用情况[J].农药科学与管理,2003,24(1):42-44
[23]Fae H.2003 Soybean weed control guide[J].Soybean Degist,2003,63(3):1-18
[24]张跃进,黄辉.我国农田化学除草历史回顾与发展对策[C],第六次全国杂草科学学术研讨会论 文集.桂林:广西民族出版社,1999:15-19
[25]张玉聚,孙化田,王春生.除草剂及其混用与农田杂草化学防治[M].北京:中国农业科技出版社,2000:159
[26]王险峰.进口农药应用手册[M].北京:中国农业出版社,2000
[27]黄春艳,陈铁保,王宇,等.28种除草剂对大豆的安全性及药害研究初报[J].植物保护,2003,29(1):31-34
[28]赵云和,张子丰,孙利.咪草烟土壤残留对后茬水稻的影响[J].农药,2006,45(3):189-190
[29]周顺启,于凤瑶,张代军,等.大豆不同耕作方法对化学除草效果的影响[J].大豆通报,2003,(6):7
[30]中华人民共和国农业部农药检定所.农药电子手册[EB].http://www.Chinapest-icide.gov.cn.2006-09-20.
[31]冯维卓.中国农田除草剂使用现状及存在问题[J].农药快讯,2001,(11):16-17
[32]刘伟,宫香余.黑龙江省大豆生产中药害现状及对策[J].大豆通报,2006,(2):37-39
[33]王焕民.对改善我国除草剂品种结构状况的思考[J].农药,2003,42(9):1-5
[34]卢向阳.几种大豆苗后除草剂与表面活性剂组合及其相互作用的研究[D].北京:中国农业大学,2001
[35]钟决龙.二苯醚类除草剂生产及大田应用现状[J].农药,2005,44(5):237-238
[36]刘长令,张运晓.国外部分农药品种在我国的知识产权保护状况[J].农药,2000,39(7):5-8
[37]王涛,贺红武,薛思佳.新颖除草剂研究进展[J].化学世界,2002,(11):608-614
[38]Alan J Tan,House William A,Parker Andrew,Canter E.Joy.transport and distribution of lindane and simazine in arivenine environment measurements in bed sediments and modeling[J].Pest Manag Sci 2004,(60)417-433
[39]匡华.大豆中苯氧羧酸除草剂的多残留检测技术研究[硕士论文].北京:中国农业大学,2006
[40]http://www.fsr.org.cn/2222.asp
[41]Gerald K Sims,Alison M Cupples.Factors controlling degradation of pesticides in soil[J].Pestic Sci,1999,(55):566-614
[42]Eiji Warabi,Kenji Usui,Yoshiyuki Tanaka,Hiroshi Matsumoto.resistance of a soybean cell line to oxyfluorfen by over production of nitochlordrial[J].Pest Manag Sci,2001,(57):743-748
[43]Liu D,Maguire R J,Lau Y.L,Pacepavicius G.J,Okamura H,Aoyama I.Factors Affecting Chemical Biodegradation,John Wiley & Sons,Inc.2000:476-438
[44]Gavrilescu M.Fate of pesticides in the environment and its bioremediation Eng.Life Sci,2005,(5):497-526
[45]Delinsky D.Amy,Bruckner V.James and Bartlett G.Michael.A review of analytical methods for the determination of trichloroethylene and its major metabolites chloral hydrate,trichloroacetic acid and dichloroacetic acid[J].Biomed.Chromatogr,2005,(19):617-639
[46]Sabine von Wiren-Lehr,Dieter Werner E.Komoa,Glagen,Heinrich Sandermann,JrIrene Scheunert.Mineralization of and its[~(14)C]Glyphosate Plant-Associated Residues in Arable Soils Originating from Different Farming Systems[J]. Pestic. Sci,1997,(51):436-442
[47] Rodrguez J, Mellado M., Corredor M. C., Pospil L, Hromadova M. Electrochemical. Reduction of Pyridinic Herbicides Picloram and Clopyralid on a Mercury Pool Electrode [J]. Electroanalysis, 2005,17(11):979-984
[48] Benedikt Gra β .Helmut Mayer, Jurgen Nolte, Gudrun Preu β , Ninette Zullei-Seibert. Studies on the metabolism of hydroxybenzonitrile herbicides:I. Mass spectrometric identification [J]. Pest Manag Sci,2000,(56):49-59
[49] Dayan E. Franck, Duke O.Stephen, Weete D.John Hancock H. Gary. Selectivity and Mode of Action of Carfentrazone-ethyl, a Novel Phenyl Triazolinone Herbicide [J]. Pestic. Sci, 1997,(51):65-73
[50] Dewez David, Marchand Mathieu, Eullaffroy Philippe, Popovic Radovan. Evaluation of the Effects of Diuron and Its Derivatives on Lemna gibba Using a Fluorescence Toxicity. Index Wiley Periodicals, Inc.2002 :493-501
[51] Avila A Liuis ,Massey H Joseph, Senseman A Scott, Armabrust L Kevin. Imazethapyr aqueous photolysis reaction quantum yield and hydroxyl radical rate constant [J]. J Agric Food Chem, 2006,(54):2635-2639
[52] Schneiderheinze J.M., Armstrong D.W., Berthod A. Plant and Soil Enantioselective Biodegradation of Racemic Phenoxyalkanoic Herbicides [J]. Chirality, 1999,(11 ):330-337
[53] Johnson Andrew.C, White Craig, Bhardwaj Clal, Dixon Andy, the ability of indigenous micro-organisms to degrade isoproputron atrazine and mecrop within aerobic UK aquifer system [J]. Pest Manag Sci,2003,(59): 1291-1302
[54] Babczinski Peter. Plant cell cultures as a model for the biochemistry of crop selectivity [J]. Pestic Sci, 1999,(55):633-675
[55] John PH Reade, Andrew H Cobb. Purification, characterization and comparison of glutathione S-transferases from black-grass (Alopecurus myosuroides Huds) biotypes [J]. Pestic Sci, 1999,(55):993-999
[56] Piutti Se'verine, Marchand Anne-Laure, Lagacherie Bernard, Fabrice Martin-Laurent and Guy Soulas. Effect of cropping cycles and repeated herbicide applications on the degradation of diclofopmethyl, bentazone, diuron, isoproturon and pendimethalin in soil [J]. Pest Manag Sci 2002,(58):303-312
[57] Pearson Robert, Godley Andrew, Carter Elise Investing the in situ degradation of atrazine in groundwater [J]. Pest Manag Sci 2006,(62):299-306
[58] Pirkko Laitinen, Katri Siimes, Liisa Eronen. Fate of the herbicides glyphosate glufosinate-ammonium, phenmedipham, ethofumesate and metamitron in two finnish arable soils [J]. Pest Manag Sci, 2006,(62):473-496
[59] Arregui Maria, Lenardon Argelia, Sanchez Daniel, Maitre L Maria, monitoring glyphosate residues in transgenic glyphosate-resist soybean [J]. Pest Manag Sci,2003,(60): 163-166
[60] 刘爱菊,朱鲁生,王军,孙瑞莲,林爱军．除草剂阿特拉津的环境毒理研究进展[J]．土壤与环境 2002,11(4):405-408
[61]Huang Sung-Ben,Thomas J Mayer,Yorkley A Robbert,Perez Rolando.Direct aqueous injection liquid chromatography/electropray ionization-mass spectrometry/mass spectrometry analysis of water for atrazine,simazine and their chlorotriazine metabolites[J].J.Agri Food Chem,2006,(40):122-125
[62]Quivet Etienne,Faure Rene,Geroges Joseph,Passe Jean-Qiiver.Photochemical degradation of imazamox in aqueous solution influence of metal ions and anionic species on the ultraviolet photolysis[J].J Agric Food Chem,2006,(54):3641-3645
[63]Kim Jim,Liu Kwang-Hueon,Kang Seung-Hun,Koo Suk-Jin.Degradation of the sulfonylurea herbicide LGC-42153 in flooded soil[J].Pest Manag Sci,2003,(59):1037-1042
[64]Patrizia Morrica,Paola Fidente and Serenella Seccia.Identification of photoproducts from imazosulfuron by HPLC[J].Biomed.Chromatogr,2004,(18):450-456
[65]苏少泉.除草剂的代谢与新品种创制[J].农药,2001,40:(9)1-3
[66]Jean Rouchoud,Marc Metsue,Michel Van Himme,Robent Bulke.Soil of metazuchlor in agronomic and vegetable crop fields[J].Weed Science,1992,(38):713-721
[67]苏少泉,滕春红,王春林.欧盟对农药的重新评定与我国除草剂品种发展[J].农药,2004,43(9):385-388
[68]Bowner,K H.Atrazine persistence and toxicity in two irrigated soils of Australia[J].Aus J Soil Res,1991,29:339-350
[69]Friesel P,Milde G,Stock R,et al.Impact of agricultural pesticide application on ground water in western Germany[A].In Proc 13th Congr.International Soil Sci,[C].Hamburg,1986:856-871
[70]Loch J P G,Van Dijk Looyard A,Zoetman B C.Organics in ground water[A].Proc.IAWPRC Conf [C].Guildford U K,1989,1:39-54
[71]Yassir A,Lagacherie B,Houots,et al.Microbial aspects of atrazine biodegradation in relation to history of soil treatment[J].Pestic Sci,1999,55:779-809
[72]Pick F E,Van Dyk L P,Botha E.Atrazine in ground and surface water in maize prod-uction areas of the transvaal[J].South Africa Chemosphere,1992,25:335-341
[73]Wehje G R,Spalding R F,Burnside O C,et al.Biological significance and fate of atra-zine under aquifer conditions[J].Weed Sci,1983,31:610-618
[74]Pensabene J W,Fiddler W,Donoghue D J.Supercritical fluid extraction of atrazine and other triazine herbicide from fortified and incurred eggs[J].J Agric Food Chem,2000,48:1668-1672
[75]杜柳涛,邬惠琼,杨杏芬,等.氟乐灵对大鼠肝、肾微粒体酶的影响[J].中国职业医学,2000,27(5):16-18
[76]Szekacs A,Trummer N,Adanyi N,et al.Developmentof a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[77]Heinrich Sandermann Jr.Bound and unextractable pesticidal plant residues chemical characterization and consumer exposure[J].Pest Manag Sci,2004,(60):613-623
[78]Michelangelo Anastassiades,Steven J.Lehotay.Fast and easy multiresidue method employing acetonitrile estraction/partitioning and dispersive solid-phase extraction for the Determination of Pesticide Residues in Peoduce[J].J AOAC Int,2003,(86):412-431
[79]Chu Xiao-Gang,Hu Xiao-Zhong,Yao Hui-Yuan.Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography-mass selective detection[J].J Chromatogra A,2005,(1063):201-210
[80]Vincze Adam,Yinon Jehuda.Tandem Mass Spectrometric Collision-induced Dissociation Study of in an Ion Trap s-Triazines Mass Spectrometer[J].J Mass Spectro,1997,(32):1320-1331
[81]Butz S.Heberer Th.,Stan H.J.Determination of phenoxyalkanoic acids and other acidic herbicides at the low ppt level in water applying solid-phase extraction with RP-C18 materi[J].J.Chromatogr.A,1994,(677):63-74
[82]匡华,储晓刚,侯玉霞.气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量[J].中国食品卫生杂志,2006,18(6):503-508
[83]霍江莲,李军,葛毅强,储晓刚.大豆中二硝基苯胺类除草剂多残留的气相色谱法定量检测及质谱确证[J].分析化学 2006,(34),特刊:S63-S67
[84]卫锋,董振霖,于玲.气相色谱—质谱联用法检测大米中多种苯氧羧酸除草剂[J].分析测试学报,2005,24(增刊):304-30
[85]张浩,刘伊玲,徐威.大豆中异丙甲草胺残留量分析方法研究[J].大豆科学,1998,17(1):88-90
[86]Serodio P.,Nogueira J.M.F.Multi-residue screening of endocrine disrupters chemicals in water samples by stir bar sorptive extraction-liquid resorption-capillary gas chromatography-mass spectrometry detection[J].Analytica Chimica Acta,2004,(517):21-32
[87]Toshihiro Fujii,Kazuhiro Hatanaka,Hiromi Arimoto,Yoshihiro Mitsutsuka.Surface Ionization Organic Mass Spectrometry of s-Triazine Herbicides[J].J Mass Spectr,1997,(32):408-412
[88]隋凯,李军,卫锋.固相萃取-高效液相色谱法同时检测大米中12种磺酰脲类除草剂的残留[J].色谱,2006,24(1):152-156
[89]祁彦,占春瑞,张新忠,杨强.高效液相色谱法测定大豆中13种三嗪类除草剂多残留量[J].分析化学,2006,(34):787-790
[90]祁彦,李淑娟,占春瑞,彭涛.高效液相色谱/质谱法测定大豆中磺酰脲类除草剂多残留量的研究[J].分析化学,2004,(32):1421-1425
[91]Schroder H F R.Mass spectrometric detection and identification of polar pesticides and their degradation products -a comparison of different ionzation method[J].J Environmental Monitoring and Assessment,1997,(44):503-513
[92]Clowers H.Brian,Steiner E.Wes,Dion M.Heather,Matz M.Laura,Tam Maggie,Tarver E.Edward,Hill H.Herbert Evaluation of Sulfonylurea Herbicides Using High Resolution Electrospray Ionization Ion Mobility Quadrupole Mass Spectrometry[J].Field Analytical Chemistry And Technology,2001,5(6):302-312
[93]Hidalgo C,Sancho J V,Hernandez F.Trace determination of triazine herbicides by means of coupled column liquid chromatography and large volume injection[J].Analytica Chimica Acta,1997,(338):223-229
[94]Giuseppe Ascenzo,Alessandra Gentili,Stefano Marchese.Optimization of High Performance Liquid Chromatography/Mass Spectrometry Apparatus for Determination of Imidazolinone Herbicides in Soil at Levels of a Few PPB[J].Rapid Commun.Mass Spectrom,1998,(12):1359-1365
[95]Carmen Molins,Elbert A.Hogendoorn,Ellen Dijkman,Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection[J].J Chromatogra A,2000,(869):487-496
[96]Renato Zanella,Ednei G.Prime,FabioF.Goncalves.Development and validation of a high-performance liquid chromatographic procedure for the determination of herbicide residues in surface and agriculture waters[J].J.Sep.Sci,2003,(26):935-938
[97]谢建军,朱亚红,朱嘉虹.除草剂双丙氨膦及代谢物草铵膦在土壤与桔子中的残留测定[J].农药,2003,42(8):18-20
[98]Satou Nemoto,Steven J.Lehotay.Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].J Agric.Food Chem,1998,(46):2190-2199
[99]许艇,邵晓龙,李季.除草剂2,4-D特异性多克隆抗体的制备及鉴定[J].生物技术2003,13(4):20
[100]施海燕,吴慧明,程敬丽等.2甲4氯人工抗原的合成与鉴定[J].农药学学报,2004,6(2):20-24
[101]Komarova NV,Kartsova LA.Optimizing Separation Conditions for Chlorophenoxycarboxylic Acid Herbicides in Natural and Potable Water Using Capillary Zone Electrophoresis[J].Anal Chem,2002,57(7):644-650
[102]Komarova NV,Kartsova LA.Determination of Herbicides of the Chlorophenoxycarboxylic Acid Type in Natural and Drinking Water by Capillary Zone Electrophoresis[J].Russian Journal of Applied Chemistry,2003,76(2):238-243
[103]Zhao Jing,Yi Guo-Xiang,He Su-Ping,Wang Bao-Min.Development of a monoclonal antibody -based enzyme-linked immunosorbent assay for the herbicide chlorimuron-ethyl[J].J Agric Food Chem,2006,(54):4948-4953
[104]Yazynina E.V.,Zherdev A.V.,Eremin S.A.,Popova V.A.,and Dzantiev B.B..Development of Enzyme Immunoassays for the Herbicide Chlorsulfuron[J].Applied Biochemistry and Microbiology,2002,38(1):9-14
[105]Dzantiev B.B,Yazynina E.V,Zherdev A.V.Determination of the herbicide chlorsulfuron by amperometric sensor based on separation-free bienzyme immunoassay[J].Sensors and Actuators B:Chemical,2004,98(2-3):254-261
[106]Yulaev M F,Sitdikov R A,Dmitrieva N M.development of a potentiometric immunosensorfor herbicide simazine and its application for food testing[J].Sensors and Actuators B,2001,(75):129-135
[107]Julia Yakovleva,Anatoly V.Zherdev,Valentina A.Popova,Sergei A.Eremin,Boris B.Dzantiev.Production of antibodies and development of enzyme-linked immunosorbent assays for the herbicide butachlor[J].Analytica Chimica Acta,2003,(491):1-13
[108]Francois MG Laurent,Rene Scalla.Metabolism and cell wall incorporation of phenoxyacetic acid in soybean cell suspension culture [J]. Pestic Sci,1999,(55):3-10
[109] http://www.cac.org.cn/
[110] E. Michael Thurman, Imma Ferrer. Amadeo Rodriguez Fern'andez-Alba[J]. J.Chromatogr A,2005, 1067:127-134
[111] E. Barcero-Barrachina, E. Moyano, M.T. Galceran [J]. J. Chromatogr A, 2004,1054:409-418
[1]Andras Szekacs,Nikoletta Trummer,Nora Adanyi et al.Development of a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[2]http://forum.globalimporter.net/view_topic/N11101105-26741-1.htm
[3]花日茂,汤锋,岳永德.甲基对硫磷、三唑酮和氟乐灵的同柱气相色谱分析[J].农药,1995,34(3):67-70
[4]黄灵芝,戴华,李拥军等.高效液相色谱法测定荞头中氟乐灵残留量[J].食品科学,2004,25(7):151-153
[5]赵凌菲,于春睿,赵国琴等.二甲戊乐灵的气相色谱分析[J].农药,1998,37(7):18-19
[6]祁彦,李淑娟,占春瑞等.高效液相色谱—质谱法测定大豆中磺酰脲类除草剂多残留量的研究[J].分析化学,2004,32:1436-1440
[7]Angel D'amato,Isabelia Semerabo,Carlo Bicchi.Simultaneous Determination of Linuron and Trifluralin Residues in Carrots and Their Pulp by Liquid Chromatography and Gas Chromatography[J].Journal of AOAC international,1993,76(3):657
[8]J.Engebretson,G.Hall,M.Hengel et al.Analysis of Pendimethalin Residues in Fruit,Nut,Vegetables,Grass,and Mint by Gas Chromatography[J].J.Agric.Food.Chem,2001,49:2198-2206
[9]Thomas A.Pressley,James E.Longbottom.The determination of dinitroaniline pesticides in industrial and municipal waste water.National technical information service,NO:PB82 156035
[10]Sheldon D.,West,Jack H.,Weston,Edgar W.,Day,JR.Gas Chromatographic Determination of Residue Level of the Herbicide Trifluralin,Benefin,Ethalfluralin,and Isopropalin in soil with Confirmation by Mass Selective Detection.[J].Assco.Of anal.Chem.1998,71(6):1082～1085
[11]Fuyu Guan,Kanako Watanabe,Akira Ishii et.Headspace solid-phase microextraction and gas chromatographic determination of dinitroaniline herbicides in human blood,urine and environmental water[J].Journal of Chromatography B,1998,714:205-213
[12]周培,陆贻通,伊雄海等.花生中氟乐灵农药残留的优化气相色谱测定法[J].上海交通大学学报,2003,21(3):205-207
[13]Julie Fillion,John Thorp.Multi-Pesticide Residue Analysis Utilizing SIM GC/MSD[J].HEWLETT PACKARD Gas-Phase Application Note,1995:228-348
[14]Akiko Tanable,Hideko Mitobe,Kuniki Kawaka et al.Monitoring of Herbicide in River water by gas chromatography-mass spectrometry and solid-phase extraction[J].Journal of chromatography A,1996,754:159-168
[15]Darcy D.Shackelford,Ron W.McCormick,Sheldon D.West et al.Determination of Ethalfluralin in Canola seed,Meal,and Refined Oil by Capillary Gas Chromatography with Mass Selective Detection[J].J.Agric.Food.Chem,2000,48:4422-4427
[16]Paolo Cabras,Marinella Melis.High-performance liquid chromatographic determination of dinitroaniline herbicides in soil and water[J].Journal of chromatography,1991,585:164-167
[17]Patrizia Vitali,Emanuela Venturini,Critina Bonora et al.Determination of triazines and dinitroanilines in waters by high-performance liquid chromatography after solid-phase extraction[J].journal of chromatography A,1994(660):219-222
[18]N.ruiz de erenchun,M.A.goicolea,Z.gomez de balugera et al.Determination of herbicide by reductive amperometric detection in liquid chromatography[J].Journal of chromatography A,1997,763:227-235
[19]Sibel Topuz,Gul Ozhan,Buket Alpertunga.Simultaneous determination of various pesticides in fruit juices by HPLC-DAD[J].Food Control,2005,16:87-92
[20]唐英章.现代食品安全检测技[M].北京:科学出版社,2004年9月
[21]Timothy M.,Fitzpatrick,Connie C.,Gehrig.Simultaneous Determination of Benefin and Trifluran in Pesticide Formulations by Gas Chromatography[J].J.ASSOC.OFF.ANAL.CHEM,1990,73(6):981-982
[22]张宇,范志先,许允成等.气质联用法测定二甲戊灵在马铃薯及土壤中的残留研究[J].吉林农业大学学报,2005,27(3):315-318
[23]朱鲁生,王军,谢慧等.二甲戊乐灵在土壤中的残留分析[J].农药.2004,43(11):512-514
[24]黄雅丽,毛黎娟,吴慧明等.二甲戊乐灵在甘蓝及土壤中的残留及消解动态研究[J].农业环境科学学报,2004,23(6):1147-1150
[25]Geoffrey B.Downer,Martin Hall,David N.B.Mallen.Determination of benefin and trifluralin residues by quantitative Gas-Liquid chromatography/Mass Spectrometry[J].J.Agric.Food Chem,1976,24(6):1223-1225
[26]Gyongyver Hegedus,Ivan Belai,Andras Szekacs.Development of an enzyme-linked Immunosorbent assay(ELISA) for the herbicide trifluralin[J].Analytica Chimica Acta,2000,421:121-133
[27]Seydou Traore,Jean-Jacques Aaron.Analysis of trifluralin and other dinitroaniline herbicide residues by zero-order and derivative ultraviolet spectrophometry[J].ANALYSIST,MAY 1989,VOL 114:609-613
[28]Andras Szekacs,Nikoletta Trummer,Nora Adanyi et al.Developmentof a non-labeled immunosensor for the herbicide trifluralin via optical waveguide lightmode spectroscopic detection[J].Analytica Chimica Acta,2003,487:31-42
[29]Ludwig Huber,Validation of Analytical Methods:Review and Strategy,LC/GC International,July 2001
[1]刘长令主编.《世界农药大全-除草剂卷》[M].北京化学工业出版社,2002
[2]中国植物保护网http://www.ipmchina.net《21世纪除草剂发展展望》
[3]http://www.pmra-arla.gc.ca.2,4-Dichlorophenoxyacetic Acid Recent Developments
[4]Tibor Cserhati,Esther Forgacs.Phenoxyacetic acids:separation and quantitative determination[J].J Chromatogr.B,1998,717:157-178
[5]Joanna Davies,John Caseley.Herbicide safeners:a review[J].J Pestic Sci,1999,55:1043-1058
[6]http://www.bml.de/englisch/pflanzenschutz/risk3-1.htm Risk reduction in the field of plant protection products in Germany.Federal Ministry of Food,Agriculture and Forestry(FMFAF)(1998).
[7]出入境检验检疫行业标准SN0661-1997,粮谷中2,4,5-T的检测
[8]出入境检验检疫行业标准SN0687-1997,粮谷油籽中禾草灵的检测
[9]出入境检验检疫行业标准SN0195-1993,肉和肉制品中2,4-D的检测
[10]出入境检验检疫行业标准SN/T-1392-2004,肉和肉制品中MCPA,MCPB的检测
[11]http://www.fsr.org.cn食品安全限量、方法
[12]林维宣.各国食品中农药残留兽药残留限量规定(第三版)[M].大连,大连海事大学出版社,2002,28-209
[13]侯宇凯,侯松嵋等.拓宽气相色谱和高效液相色谱分析应用范围的有效途径—化学衍生法[J].化工标准·计量·质量,2001,5:29-31
[14]Moustapha Belmouden,Ali Assabbane,Yhia Ait Ichou.Adsorption characteristics of a phenoxy acetic acid herbicide on activated carbon[J].Environ Monit,2000,2:257-260
[15]S.Butze,Th.Heberer,H.-J.Stan Determination of phenoxyalkanoic acids and other acidic herbicides at the low ppt level in water applying solid-phase extraction with RP-C_(18) material[J].Chromatogr.A,1994,677:63-74
[16]USA EPA method 8041A Phenols By Gas Chromatography
[17]P.Cabras,C.Tuberoso,M.Melis,et al.Multiresidue method for pesticide determination in wine by high-performance liquid chromatography[J].J.Agric.Food Chem,.1992,40:817-819
[18]Balinova.Multiresidue determination of pesticides in plants by high-performance liquid chromatography following gel permeation chromatographic clean-up[J].J Chromatogr A,1998,823:11-16
[19]Aldo Lagana,Giovanna Fago,Alessondra Marinob.Liquid chromatography mass spectrometry tandem for multiresidue determination of selected post-emergence herbicides after soil column extraction[J].J Analytica Chimica Acta,2000,(415):41-56
[20]Paul R.Loconto.Isolation and recovery from water of selected chlorophenoxy acid herbicides and similar weak acid herbicides by solid-phase extraction HPLC and photodiode array detection[J].J liquid chromatogr,1991,14,7:1297-1314
[21]M.J.Incoruia.Mattina determination of chlorophenoxy acids using high performance liquid chromatography-particle beam mass spectrometry[J].J.Chromatogra,1991,542:385-395
[22]B.Rene,Geerdink,Paul G.M.Kieuhuis fast screening method for eight phenoxy acid herbicides-optimization procedures for flow-injection analysis-thermospray tandem mass spectrometry[J].J.Chromatogra,1993,647:329-339
[23]H.FR.Schroder.Mass spectrometric detection and identification of polar pesticides and their degradation products-a comparison of different ionzation method[J].Environmental Monitoring and Assessment,1997,44:503-513
[24]J.Patsias,E.Papadopoulou-Mourkidou.Rapid method for the ananlysis of a variety of chemical classes of pesticides insurface and ground waters by off-line solid-phase extraction and gas chromatography-ion trap mass spectrometry[J].J.Chromatogra,1996,740:83-98
[25]Karl-Heinz Bauer,Thomas P.Knepper,Anke Maes Analysis of polar organic micropollutants in water with ion chromatography-electrospray mass spectrometry[J].J.Chromatogr A,1999,837:117-128
[26]Tibor Cserhati,Esther Forgacs,Zdenek Deyl.Chromatographic determination of herbicide residues in various matrices[J].J.Biomed.Chromatogr,2004,18:350-359
[27]Stefano Marchese,Daniela Perret,Alessandra Gentili,et al.Determination of phenoxyacid herbicides and their phenolic metabolites in surface and drink water[J].Rapid Commun,Mass Spectrum,2002,16:134-141
[28]O.Pozo,E.Pitarch,J.V.Sancho,F.Hernandez.Determination of the herbicide 4-chloro-2-methylphenoxyacetic acid and its main metabolite,4-chloro-2-methylphenol in water and soil by liquid chromatography-electrospray tandem mass spectrometry[J].J.Chromatogr A,2001,923:75-85
[29]Su Tiana,Kozo Nakamurab,Tong Cuic,High-performance liquid chromatographic determinationof phenolic compounds in rice[J].J.Chromatogr A,2005(1063):121-128
[30]Adriana Farran,Santiago Ruiz.Application of solid-phase extraction and micellar electrokinetic capillary chromatography to the study of hydrolytic and photolytic degradation of phenoxy acid and phenylurea herbicides[J].J.Chromatogr.A,2004,1024:267-274
[31]N.V.Komarova,L.A.Kartsova.Optimizing Separation Conditions for Chlorophenoxycarboxylic Acid Herbicides in Natural and Potable Water Using Capillary Zone Electrophoresis[J].Anal Chem,2002,57(7):644-650
[32]N.V.Komarova,L.A.Kartsova.Determination of Herbicides of the Chlorophenoxycarboxylic Acid Type in Natural and Drinking Water by Capillary Zone Electrophoresis[J].Russian Journal of Applied Chemistry,2003,76(2):238-243
[33]Satou Nemoto,Steven J.Lehotay.Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].Agric.Food.Chem 1998,46:2190-2199
[34]蔡春平,王丹红,吴灵威等.苯氧羧酸类除草剂的毛细管电泳手性拆分研究[J].检验检疫科学,2004,14(6):23-25
[35]A.W.Garrison,P.Schmitt,A.Kettrup.Separation of phenoxy acid herbicides and their enantiomers by high-performance capillary electrophoresis[J].Chromatogr A,1994,684:317-327
[36]文岳中,蔡喜运,马云等.衍生化-手性毛细管色谱分离和测定水中的2,4-滴丙酸[J].分析化学32(11):1492-1494
[37]Gyrd-Hansen,N.and S.Dalgaard-Mikkelsen.The effect of phenoxy-herbicides on the hatchability of eggs and the viability of the chicks[J].Acta Pharmacol.Toxicol 1974,35:300-308
[38]许艇,邵晓龙,李季等.除草剂2,4-D特异性多克隆抗体的制备及鉴定[J].生物技术,2003,13(4):20-21
[39]施海燕,吴慧明,程敬丽等.2-甲-4-氯人工抗原的合成与鉴定[J].农药学学报,2004,6(2):20-24
[1]刘长令主编.世界农药大全-除草剂卷[M].北京,化学工业出版社,2002年
[2]海外传真.农药,2003,42(7):47
[3]林维宣.各国食品中农药残留兽药残留限量规定[M],大连,大连海事大学出版社,2002
[4]Prince J.L.,Guinivan R.A.Analysis of chlorimuron ethyl in crops by high performance liquid chromatography[J].J.Agric.Food Chem,1988,36:63-69
[5]Galletti G.C.,Bonetti A.High performance liquid chromatographic determination of sulfonylureas in soil and water[J].J.Chromtogr.A.,1995,692:27-37
[6]Menne J.H.,Janowitz K.Comparison of capillary electrophoresis and liquid chromatography for determination of sulfonylurea herbicides in soil[J].J.AOAC Internal.,1999,82(6):1534-1541
[7]Yumi A.,Naoki Y.and Masahiko T.Application of Multiresidue Screening Method to Pesticides for which Establishment of Maximum Residue Limits was Inquired in F.Y.1997[J].J.Food Hyg.Soc.Japan,2002,33:114-119
[8]Krynitsky J.A.Determination of sulfonylurea herbicides in grains by capillary electrophoresis[J].J.AOAC Int.,1997,80(2):392-340
[9]Nemoto S,Lehotay S.J.Analysis of multiple herbicides in soybeans using pres-surized liquid extraction and capillary elec-trophoresis[J].J.Agric.Food Chem,1998,46:2190-2199
[10]衣先众,姜得峰等.除草剂在大豆田应用研究[J].莱阳农学院学报,1999,16(1):25-27
[11]王晴 赵长山等.除草剂绿黄隆在小麦及大豆植株中残留分析方法的研究[J].化学工程师,1999,1:18-19
[12]默涛,张少军等.三氟羧草醚在大豆、茎叶及土壤中的残留分析方法研究[J].河北农业科学,1993,4:17-19
[1]刘长令.三嗪类除草剂的创制经纬[J].农药,2002,41(4):46
[2]孔志明,吴庆龙、黄健等.除草剂环嗪酮的毒性研究[J].农药,1994,33(5):31
[3]张一宾.世界三嗪类除草剂的发展概况.农药论坛
[4]朱忠林,单正军,蔡道基等.环嗪酮对生态环境影响评价研究.环境科学进展[J].1991,33(5):31
[5]王筱芬,刘毅,陶玉珍等.氰草津的毒理学研究[J].农药,1997,36(8):28-29
[6]潘洪吉,张群峰,李常平.苯嗪草酮原药的液相色谱分析方法[J].农药科学与管理,2000,21(2):4-5
[7]陈玲,郜洪文,董丽娴等.固相萃取—高效液相色谱法测定环境水样中的三嗪类化合物[J].色谱,2006,24(3):267-270
[8]任晋,黄翠玲,赵国栋等.固相萃取—高效液相色谱—质谱联机在线分析水中痕量除草剂[J].分析化学研究报告,2001,29(8):876-880
[9]刘长令.世界农药大全:除草剂卷[M].北京:化学工业出版社,2002
[10]苏少泉.酰胺类除草剂评述[J].农药,2002,41(11):1-5
[11]Institute for the Control of Agrochemicals,Ministry of Agriculture,P.R.China.Handbook of Practi cal Methods for the Determination of Pesticide Residues,Vol.1.Beijing:China Agriculture Publish ing House,1995
[12]黄宝华,叶秀薇.丙草胺的气相色谱分析[J].农药,1997,36(6):33-34
[1]Hidalgo C,Sancho J V,Hernandez F.Trace determination of triazine herbicides by means of coupled-column liquid chromatography and large volume injection[J].Analytica Chimica Acta,1997,338:223-229
[2]Giuseppe Ascenzo,Alessandra Gentili,Stefano Marchese.Determination of arylphenoxypropionic herbicides in water by liquid chromatography-electrospray mass spectrometry Rapid Commun[J].Mass Spectrom,1998,12,1359-1365
[3]Carmen Molins,Elbert A.Hogendoorn,Ellen Dijkman.Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection[J].J Chromatogra A,2000,869:487-496
[4]Renato Zanella,Ednei G.Prime,Fabio F.Goncalves,Determination of total arsenic by batch hydride generation atomic absorption spectrometry in injectable drugs containing high levels of Sb(V) as N-methylglucamine antimonate[J].J.Sep.Sci.,2003,26:.935-938
[5]Serodio P.,Nogueira J.M.F.Multi-residue screening of endocrine disrupters chemicals in water samples by stir bar sorptive extraction-liquid desorption-capillary gas chromatography-mass spectrometry detection[J].Analytica Chimica Acta,2004,517:21-32
[6]卫锋,董振霖,于玲等.气相色谱-质谱联用法检测大米中多种苯氧羧酸除草剂[J].分析测试学报,2005,24(增刊):304-306
[7]隋凯,李军,卫锋等.固相萃取-高效液相色谱法同时检测大米中12种磺酰脲类除草剂的残留[J].色谱,2006,24(1):152-156.
[8]张浩,刘伊玲,徐威等.大豆中异丙甲草胺残留量分析方法研究[J].大豆科学,1998,17(1):88-90.
[9]Satoru Nemoto,Steven J.Lehotay,Analysis of multiple herbicides in soybeans using pressurized liquid extraction and capillary electrophoresis[J].J.Agric.Food.Chem.,1998,46:2190-2199.
[1] http://www.cac.org.cn/
[2] B.A. Mamyrin. Time-of-flight mass spectrometry (concepts, achievements, and prospects) Int. [J]. Mass Spectrom, 2001,206:251-266
[3] E.M. Thurman, Imma Ferrer. Accurate mass analysis of ethanesulfonic acid degradates of acetochlor and alachlor using high-performance liquid chromatography and time-of-flight mass spectrometry [J]. J.Chromatogr A, 2002,957:3-9
[4] E. Michael Thurman, Imma Ferrer, Jerry A. Zweigenbaum. Discovering metabolites of post-harvest fungicides in citrus with liquid chromatography/time-of-flight mass spectrometry and ion trap tandem mass spectrometry [J]. J.Chromatogr A, 2005,1082: 71-80
[5] Emoto S, Steven JL. Agricultural pesticide residues in oysters and water from two Chesapeake bay tributaries[J]. J.Agric Food Chem, 1998,46: 2190-2199