Sin-QuEChERS结合UPLC-MS/MS同时检测茶叶中10种有机磷农药残留
|
摘要
基于茶叶样品基质复杂的特点,采用简易的基质分散净化(Sin-QuEChERS)法对样品前处理技术加以改进,并结合超高效液相色谱-串联质谱(UPLC-MS/MS)技术,建立了同时检测茶叶中10种有机磷农药残留的分析方法。与传统的样品预处理方法相比,该方法在保证重复性和稳定性的前提下,具有操作简单、省时省力、普适性好、灵敏度高等优点。在优化的Sin-QuEChERS方法提取净化条件和UPLC-MS/MS检测条件下,可将样品前处理时间控制在10 min以内,使每个样品的分析在0.5 h内完成。结果表明:10种有机磷农药的线性范围为1～500μg/L,检出限为0.08～1.38μg/kg,定量限为0.27～4.60μg/kg;在不同的加标水平下,平均回收率在71.6%～115.0%之间,RSD小于14.5%,与国家标准方法的检测结果接近。将该方法应用于检测空白茶叶加标样品和20种市售茶叶中有机磷农药,验证了方法的可行性。该研究可为快速、简易、准确地评价茶叶中多种有机磷类农药的质量安全提供方法参考。
Based on the characteristics of tea samples, a method was established for simultaneously detection of 10 organophosphorus pesticides residues(dimethoate, omethoate, phosemet, malathion, dipterex, dichlorovos, quinalphos, demeton, methamidophos, monocrotophos). In this method, a novel pretreatment method of Sin-QuEChERS was used for extraction and purification, and ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) technology was used for detection. In view of the strong matrix effect of tea samples and the characteristics of organophosphorus pesticide decomposition with heat, a packing column filled with PSA, C18, carbon multiwalled nanotubes(CMWNTs) was applied in the Sin-QuEChERS methods. After an ordinary extraction by acetonitrile, vortex oscillation and centrifugation, the purification of chlorophyll, lutein and tea polyphenols in tea leaves was processed with a simple pressing of the Sin-QuEChERS packing column. The purified solution can be directly injected into the detector. This Sin-QuEChERS method can improve the removal effect of matrix interference by SPE, improve the purification effect of pigments, lipids and some sugar sterols, and reduce the interference of chromatogram. Compared with other extraction and purification methods, it has the advantages of simple operation, obvious purification effect on impurities, less adsorption on pesticides and accurate results, and can greatly shorten the analysis time. At the same time, because this method does not involve heating and other links, it is suitable for temperature decomposition of organophosphorus pesticides extraction and purification operation, and is able to improve the accuracy of organophosphorus pesticides detection results. In the optimized Sin-QuEChERS methods and UPLC-MS/MS detection conditions, the preprocessing time can be controlled within 10 min, so that the analysis time of a sample can be completed within the 0.5 h. The linear range of 10 organophosphorus pesticides is 1-500 μg/L. The limit of detection(LOD) is 0.08-1.38 μg/kg, and the limit of quantity(LOQ) is 0.27-4.60 μg/kg. The recoveries are 71.6%-115.0% and RSDs of different spiking levels are less than 14.5%. Compared with the traditional sample pretreatment method, the new developed method has the advantages of simple operation, time-saving, good universality and high sensitivity with the premise of ensuring repeatability. The method was applied for the detection of organophosphorus pesticides in standard addition of blank tea samples and 20 kinds of tea, which proved the feasibility and importance of the method. This method provides a new way to evaluate the quality and safety of tea more quickly, simply, cheaply and accurately.
Based on the characteristics of tea samples, a method was established for simultaneously detection of 10 organophosphorus pesticides residues(dimethoate, omethoate, phosemet, malathion, dipterex, dichlorovos, quinalphos, demeton, methamidophos, monocrotophos). In this method, a novel pretreatment method of Sin-QuEChERS was used for extraction and purification, and ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) technology was used for detection. In view of the strong matrix effect of tea samples and the characteristics of organophosphorus pesticide decomposition with heat, a packing column filled with PSA, C18, carbon multiwalled nanotubes(CMWNTs) was applied in the Sin-QuEChERS methods. After an ordinary extraction by acetonitrile, vortex oscillation and centrifugation, the purification of chlorophyll, lutein and tea polyphenols in tea leaves was processed with a simple pressing of the Sin-QuEChERS packing column. The purified solution can be directly injected into the detector. This Sin-QuEChERS method can improve the removal effect of matrix interference by SPE, improve the purification effect of pigments, lipids and some sugar sterols, and reduce the interference of chromatogram. Compared with other extraction and purification methods, it has the advantages of simple operation, obvious purification effect on impurities, less adsorption on pesticides and accurate results, and can greatly shorten the analysis time. At the same time, because this method does not involve heating and other links, it is suitable for temperature decomposition of organophosphorus pesticides extraction and purification operation, and is able to improve the accuracy of organophosphorus pesticides detection results. In the optimized Sin-QuEChERS methods and UPLC-MS/MS detection conditions, the preprocessing time can be controlled within 10 min, so that the analysis time of a sample can be completed within the 0.5 h. The linear range of 10 organophosphorus pesticides is 1-500 μg/L. The limit of detection(LOD) is 0.08-1.38 μg/kg, and the limit of quantity(LOQ) is 0.27-4.60 μg/kg. The recoveries are 71.6%-115.0% and RSDs of different spiking levels are less than 14.5%. Compared with the traditional sample pretreatment method, the new developed method has the advantages of simple operation, time-saving, good universality and high sensitivity with the premise of ensuring repeatability. The method was applied for the detection of organophosphorus pesticides in standard addition of blank tea samples and 20 kinds of tea, which proved the feasibility and importance of the method. This method provides a new way to evaluate the quality and safety of tea more quickly, simply, cheaply and accurately.
引文
[1] HU J,CHEN Y,NI D.Effect of superfine grinding on quality and antioxidant property of fine green tea powders[J].LWT-Food Science & Technology,2012,45(1):8-12.
[2] KOBAYASHI M,IKEDA I.Mechanisms of inhibition of cholesterol absorption by green tea catechins[J].Food Science & Technology Research,2017,23(5):627-636.
[3] 霍丹群,付贝贝,李俊杰,杨眉,沈才洪,罗惠波,侯长军.基于液体阵列比色传感器鉴别不同茶叶的新方法[J].高等学校化学学报,2016,37(5):873-880.HUO Danqun,FU Beibei,LI Junjie,YANG Mei,SHEN Caihong,LUO Huibo,HOU Changjun.New method for identifying different teas based on liquid colorimetric sensor[J].Chemical Journal of Chinese Universities,2016,37(5):873-880(in Chinese).
[4] 张娅婷,秦广雍,孔令军,张书胜.利用亚临界丁烷分离茶树鲜叶中的阿维菌素[J].分析化学,2017,45(6):844-850.ZHANG Yating,QIN Guangyong,KONG Ling-jun,ZHANG Shusheng.Subcritical butane extraction for effective removal of abamectin in fresh tea leaves[J].Chinese Journal of Analytical Chemistry,2017,45(6):844-850(in Chinese).
[5] YUE N,KUANG H,SUN L,WU L,XU C.An empirical analysis of the impact of EU’s new food safety standards on China’s tea export[J].International Journal of Food Science Technology,2010,45(4):745-750.
[6] CHEN H P,HAO Z X,WANG Q H,JIANG Y,PAN R,WANG C,LIU X,LU C.Occurrence and risk assessment of organophosphorus pesticide residues in Chinese tea[J].Human and Ecological Risk Assessment:An International Journal,2016,22(1):28-38.
[7] ZHENG X Y,HE L J,DUAN Y J,JIANG X,XIANG G,ZHAO W,ZHANG S.Poly (ionic liquid) immobilized magnetic nanoparticles as new adsorbent for extraction and enrichment of organophosphorus pesticides from tea drinks[J].Journal of Chromatography A,2014,1 358:39-45.
[8] WU M Y C,HSU M Y,CHEN S J,HWANG D K,YEN T H,CHENG C M.Point-of-care detection devices for food safety monitoring:proactive disease prevention[J].Trends in Biotechnology,2017,35(4):288-300.
[9] KRAUSE K H,VAN THRIEL C,DE SOUSA P A,LEIST M,HENGSTLER J G.Monocrotophos in Gandaman village:India school lunch deaths and need for improved toxicity testing[J].Archives of Toxicology,2013,87(10):1 877-1 881.
[10] GB 2763—2016.食品安全国家标准-食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[11] ROSHANAK S,RAHIMMALEK M,GOLI S A H.Evaluation of seven different drying treatments in respect to total flavonoid,phenolic,vitamin C content,chlorophyll,antioxidant activity and color of green tea (Camellia sinensis or C.assamica) leaves[J].Journal of Food Science and Technology,2016,53(1):721-729.
[12] 黄田田,汤桦,董晓倩,刘松南,许雯雯,王华,宗琦.多壁碳纳米管QuEChERS-气相色谱法测定茶叶中23 种有机磷农药残留量[J].食品科学,2018,39(6):315-321.HUANG Tiantian,TANG Hua,DONG Xiaoqian,LIU Songnan,XU Wenwen,WANG Hua,ZONG Qi.Determination of 23 organophosphorus pesticide residues in tea by QuEChERS extraction with multi-walled carbon nanotubes (MWCNTs) coupled to gas chromatography[J].Food Science,2018,39(6):315-321(in Chinese).
[13] HOU X,LEI S R,QIU S,GUO L,YI S,LIU W.A multi-residue method for the determination of pesticides in tea using multi-walled carbon nanotubes as a dispersive solid phase extraction absorbent[J].Food Chemistry,2014,153:121-129.
[14] LI J X,ZHANG Z J,SUN M Y,ZHANG B L,FAN C L.Use of a headspace solid-phase microextraction-based methodology followed by gas chromatography-tandem mass spectrometry for pesticide multiresidue determination in teas[J].Chromatographia,2018,81(5):809-821.
[15] FANG Y,TIAN W,PEI F,LI P,SHAO X L,FAN Y,HU Q.Simultaneous determination of pesticide residues and antioxidants in blended oil using a liquid-liquid extraction combined with dispersive solid phase extraction method[J].Food Chemistry,2017,229:347-353.
[16] KDAIR H A,ABAS F,ZAKARIA O,ISMAIL I S,LAJIS N H.Analysis of pesticide residues in tea using accelerated solvent extraction with in-cell cleanup and gas chromatography tandem mass spectrometry[J].Analytical Methods,2015,7:3 141-3 147.
[17] 张新忠,罗逢键,张芬,刘光明,楼正云,陈宗懋.分散固相萃取净化气相色谱串联质谱法测定茶叶、西葫芦和芒果中噻螨酮和噻嗪酮残留量[J].分析化学,2012,40(11):1 686-1 692.ZHANG Xinzhong,LUO Fengjian,ZHANG Fen,LIU Guangming,LOU Zhengyun,CHEN Zongmao.Residue determination of hexythiazox and buprofezin in tea,marrow and mango by gas chromatography coupled with tandem mass spectrometry after dispersive solid phase extraction cleanup[J].Chinese Journal of Analytical Chemistry,2012,40(11):1 686-1 692(in Chinese).
[18] ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,SCHIENCK F J.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[19] 董晓倩,刘松南,刘蕊,黄田田,宗琦,王华,欧阳亚旭.QuEChERS-液相色谱-串联质谱法测定茶叶中的丁醚脲[J].食品科学,2017,38(8):244-250.DONG Xiaoqian,LIU Songnan,LIU Rui,HUANG Tiantian,ZONG Qi,WANG Hua,OUYANG Yaxu.Determination of diafenthiuron residue in tea by QuEChERS-liquid chromatography-tandem mass spectrometry[J].Food Science,2017,38(8):244-250(in Chinese).
[20] HE Z,WANG L,PENG Y,LUO M,WANG W,LIU X.Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chemistry,2015,169:372-380.
[21] RIZZETTI T M,KEMMERICH M,MARTINS M L,PRESTES O D,ADAIME M B,ZANELLA R.Optimization of a QuEChERS based method by means of central composite design for pesticide multiresidue determination in orange juice by UHPLC-MS/MS[J].Food Chemistry,2016,196:25-33.
[22] LOZANO A,RAJSKI ?,BELMONTE-VALLES N,UCLES A,UCLES S,MEZCUA M,FERNANDEZ-ALBA A R.Pesticide analysis in teas and chamomile by liquid chromatography and gas chromatography tandem mass spectrometry using a modified QuEChERS method:validation and pilot survey in real samples[J].Journal of Chromatography A,2012,1 268:109-122.
[23] 刘松南,赵新颖,董晓倩,许雯雯,赵榕.QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉[J].色谱,2015,33(11):1 205-1 209.LIU Songnan,ZHAO Xinying,DONG Xiaoqian,XU Wenwen,ZHAO Rong.Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2015,33(11):1 205-1 209(in Chinese).
[24] WU C C.Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry[J].Food Chemistry,2017,229:580-587.
[25] 董亚蕾,刘文婧,曹进,王钢力.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学,2017,9(45):1 397-1 404.DONG Yalei,LIU Wenjing,CAO Jin,WANG Gangli.Determination of 38 kinds of pesticide residues in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,9(45):1 397-1 404(in Chinese).
[26] ZHOU J,XU J J,CONG J M,CAI Z X,ZHANG J S,WANG J L,REN Y P.Optimization for quick,easy,cheap,effective,rugged and safe extraction of mycotoxins and veterinary drugs by response surface methodology for application to egg and milk[J].Journal of Chromatography A,2017,1 532:20-29.
[27] ARIAS J L O,SCHNEIDER A,BATISTA-ANDRADE J A,VIEIRA A A,CALDAS S S,PRIMEL E G.Chitosan from shrimp shells:a renewable sorbent applied to the clean-up step of the QuEChERS method in order to determine multi-residues of veterinary drugs in different types of milk[J].Food Chemistry,2017,240:1 243-1 253.
[28] 郭春景,李娜,王建忠.超高效液相色谱-串联质谱法快速测定8种蔬菜中114种农药残留[J].质谱学报,2014,35(3):279-288.GUO Chunjing,LI Na,WANG Jianzhong.Rapid detectin of 114 pesticide residues in eight vegetables by UPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2014,35(3):279-288(in Chinese).
[29] 郭春景,王建忠,郝晓莉.利用QuEChERS-UPLC-MS/MS法测定甘蓝、草莓中7种农药残留的实验条件优化探索[J].质谱学报,2013,34(2):121-127.GUO Chunjing,WANG Jianzhong,HAO Xiaoli.The condition optimization determination of multi-residue of pesticides in cabbage and strawberry by QuEChERS-UPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2013,34(2):121-127(in Chinese).
[30] ZHANG Q X.Extraction structure,extraction module,and liquid pretreatment device[P].United States Patent,2017/0326481 A1,2017-11-16.
[31] GB 23200.13—2016.食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.
[32] 王翔,宋国新,胡耀铭.GC/MS研究茶叶中拟除虫菊酯类农药残留的提取方法[J].质谱学报,2008,29(2):97-100.WANG Xiang,SONG Guoxin,HU Yaoming.Study on extaction of pyrethroid pesticide multi-residues in tea by GC/MS[J].Journal of Chinese Mass Spectrometry Society,2008,29(2):97-100(in Chinese).
[33] AOAC Official Method 2007.01.Pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[EB/OL].http://www.weber.hu/Downloads/SPE/QuEChERS/AOAC_2007_01.pdf.
[34] 庞国芳,范春林,李岩,康健,常巧英,卜明楠,金春丽,陈辉.茶叶中653种农药化学品残留GC-MS、GC-MS/MS与LC-MS/MS分析方法:国际AOAC方法评价预研究[J].分析测试学报,2012,31(9):1 017-1 030.PANG Guofang,FAN Chunlin,LI Yan,KANG Jian,CHANG Qiaoying,PU Mingnan,JIN Chunli,CHEN Hui.Determination of 653 pesticides and chemical contaminants residues in tea by GC-MS,GC-MS/MS and LC-MS/MS:the pre-collaborative study of aoac method efficiency evaluation[J].Journal of Instrumental Analysis,2012,31(9):1 017-1 030(in Chinese).
[35] SN/T 1950—2007.进出口茶叶中多种有机磷农药残留量的检测方法气相色谱法[S].北京:中国标准出版社,2007.
[2] KOBAYASHI M,IKEDA I.Mechanisms of inhibition of cholesterol absorption by green tea catechins[J].Food Science & Technology Research,2017,23(5):627-636.
[3] 霍丹群,付贝贝,李俊杰,杨眉,沈才洪,罗惠波,侯长军.基于液体阵列比色传感器鉴别不同茶叶的新方法[J].高等学校化学学报,2016,37(5):873-880.HUO Danqun,FU Beibei,LI Junjie,YANG Mei,SHEN Caihong,LUO Huibo,HOU Changjun.New method for identifying different teas based on liquid colorimetric sensor[J].Chemical Journal of Chinese Universities,2016,37(5):873-880(in Chinese).
[4] 张娅婷,秦广雍,孔令军,张书胜.利用亚临界丁烷分离茶树鲜叶中的阿维菌素[J].分析化学,2017,45(6):844-850.ZHANG Yating,QIN Guangyong,KONG Ling-jun,ZHANG Shusheng.Subcritical butane extraction for effective removal of abamectin in fresh tea leaves[J].Chinese Journal of Analytical Chemistry,2017,45(6):844-850(in Chinese).
[5] YUE N,KUANG H,SUN L,WU L,XU C.An empirical analysis of the impact of EU’s new food safety standards on China’s tea export[J].International Journal of Food Science Technology,2010,45(4):745-750.
[6] CHEN H P,HAO Z X,WANG Q H,JIANG Y,PAN R,WANG C,LIU X,LU C.Occurrence and risk assessment of organophosphorus pesticide residues in Chinese tea[J].Human and Ecological Risk Assessment:An International Journal,2016,22(1):28-38.
[7] ZHENG X Y,HE L J,DUAN Y J,JIANG X,XIANG G,ZHAO W,ZHANG S.Poly (ionic liquid) immobilized magnetic nanoparticles as new adsorbent for extraction and enrichment of organophosphorus pesticides from tea drinks[J].Journal of Chromatography A,2014,1 358:39-45.
[8] WU M Y C,HSU M Y,CHEN S J,HWANG D K,YEN T H,CHENG C M.Point-of-care detection devices for food safety monitoring:proactive disease prevention[J].Trends in Biotechnology,2017,35(4):288-300.
[9] KRAUSE K H,VAN THRIEL C,DE SOUSA P A,LEIST M,HENGSTLER J G.Monocrotophos in Gandaman village:India school lunch deaths and need for improved toxicity testing[J].Archives of Toxicology,2013,87(10):1 877-1 881.
[10] GB 2763—2016.食品安全国家标准-食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[11] ROSHANAK S,RAHIMMALEK M,GOLI S A H.Evaluation of seven different drying treatments in respect to total flavonoid,phenolic,vitamin C content,chlorophyll,antioxidant activity and color of green tea (Camellia sinensis or C.assamica) leaves[J].Journal of Food Science and Technology,2016,53(1):721-729.
[12] 黄田田,汤桦,董晓倩,刘松南,许雯雯,王华,宗琦.多壁碳纳米管QuEChERS-气相色谱法测定茶叶中23 种有机磷农药残留量[J].食品科学,2018,39(6):315-321.HUANG Tiantian,TANG Hua,DONG Xiaoqian,LIU Songnan,XU Wenwen,WANG Hua,ZONG Qi.Determination of 23 organophosphorus pesticide residues in tea by QuEChERS extraction with multi-walled carbon nanotubes (MWCNTs) coupled to gas chromatography[J].Food Science,2018,39(6):315-321(in Chinese).
[13] HOU X,LEI S R,QIU S,GUO L,YI S,LIU W.A multi-residue method for the determination of pesticides in tea using multi-walled carbon nanotubes as a dispersive solid phase extraction absorbent[J].Food Chemistry,2014,153:121-129.
[14] LI J X,ZHANG Z J,SUN M Y,ZHANG B L,FAN C L.Use of a headspace solid-phase microextraction-based methodology followed by gas chromatography-tandem mass spectrometry for pesticide multiresidue determination in teas[J].Chromatographia,2018,81(5):809-821.
[15] FANG Y,TIAN W,PEI F,LI P,SHAO X L,FAN Y,HU Q.Simultaneous determination of pesticide residues and antioxidants in blended oil using a liquid-liquid extraction combined with dispersive solid phase extraction method[J].Food Chemistry,2017,229:347-353.
[16] KDAIR H A,ABAS F,ZAKARIA O,ISMAIL I S,LAJIS N H.Analysis of pesticide residues in tea using accelerated solvent extraction with in-cell cleanup and gas chromatography tandem mass spectrometry[J].Analytical Methods,2015,7:3 141-3 147.
[17] 张新忠,罗逢键,张芬,刘光明,楼正云,陈宗懋.分散固相萃取净化气相色谱串联质谱法测定茶叶、西葫芦和芒果中噻螨酮和噻嗪酮残留量[J].分析化学,2012,40(11):1 686-1 692.ZHANG Xinzhong,LUO Fengjian,ZHANG Fen,LIU Guangming,LOU Zhengyun,CHEN Zongmao.Residue determination of hexythiazox and buprofezin in tea,marrow and mango by gas chromatography coupled with tandem mass spectrometry after dispersive solid phase extraction cleanup[J].Chinese Journal of Analytical Chemistry,2012,40(11):1 686-1 692(in Chinese).
[18] ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,SCHIENCK F J.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[19] 董晓倩,刘松南,刘蕊,黄田田,宗琦,王华,欧阳亚旭.QuEChERS-液相色谱-串联质谱法测定茶叶中的丁醚脲[J].食品科学,2017,38(8):244-250.DONG Xiaoqian,LIU Songnan,LIU Rui,HUANG Tiantian,ZONG Qi,WANG Hua,OUYANG Yaxu.Determination of diafenthiuron residue in tea by QuEChERS-liquid chromatography-tandem mass spectrometry[J].Food Science,2017,38(8):244-250(in Chinese).
[20] HE Z,WANG L,PENG Y,LUO M,WANG W,LIU X.Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chemistry,2015,169:372-380.
[21] RIZZETTI T M,KEMMERICH M,MARTINS M L,PRESTES O D,ADAIME M B,ZANELLA R.Optimization of a QuEChERS based method by means of central composite design for pesticide multiresidue determination in orange juice by UHPLC-MS/MS[J].Food Chemistry,2016,196:25-33.
[22] LOZANO A,RAJSKI ?,BELMONTE-VALLES N,UCLES A,UCLES S,MEZCUA M,FERNANDEZ-ALBA A R.Pesticide analysis in teas and chamomile by liquid chromatography and gas chromatography tandem mass spectrometry using a modified QuEChERS method:validation and pilot survey in real samples[J].Journal of Chromatography A,2012,1 268:109-122.
[23] 刘松南,赵新颖,董晓倩,许雯雯,赵榕.QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉[J].色谱,2015,33(11):1 205-1 209.LIU Songnan,ZHAO Xinying,DONG Xiaoqian,XU Wenwen,ZHAO Rong.Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2015,33(11):1 205-1 209(in Chinese).
[24] WU C C.Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry[J].Food Chemistry,2017,229:580-587.
[25] 董亚蕾,刘文婧,曹进,王钢力.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学,2017,9(45):1 397-1 404.DONG Yalei,LIU Wenjing,CAO Jin,WANG Gangli.Determination of 38 kinds of pesticide residues in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,9(45):1 397-1 404(in Chinese).
[26] ZHOU J,XU J J,CONG J M,CAI Z X,ZHANG J S,WANG J L,REN Y P.Optimization for quick,easy,cheap,effective,rugged and safe extraction of mycotoxins and veterinary drugs by response surface methodology for application to egg and milk[J].Journal of Chromatography A,2017,1 532:20-29.
[27] ARIAS J L O,SCHNEIDER A,BATISTA-ANDRADE J A,VIEIRA A A,CALDAS S S,PRIMEL E G.Chitosan from shrimp shells:a renewable sorbent applied to the clean-up step of the QuEChERS method in order to determine multi-residues of veterinary drugs in different types of milk[J].Food Chemistry,2017,240:1 243-1 253.
[28] 郭春景,李娜,王建忠.超高效液相色谱-串联质谱法快速测定8种蔬菜中114种农药残留[J].质谱学报,2014,35(3):279-288.GUO Chunjing,LI Na,WANG Jianzhong.Rapid detectin of 114 pesticide residues in eight vegetables by UPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2014,35(3):279-288(in Chinese).
[29] 郭春景,王建忠,郝晓莉.利用QuEChERS-UPLC-MS/MS法测定甘蓝、草莓中7种农药残留的实验条件优化探索[J].质谱学报,2013,34(2):121-127.GUO Chunjing,WANG Jianzhong,HAO Xiaoli.The condition optimization determination of multi-residue of pesticides in cabbage and strawberry by QuEChERS-UPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2013,34(2):121-127(in Chinese).
[30] ZHANG Q X.Extraction structure,extraction module,and liquid pretreatment device[P].United States Patent,2017/0326481 A1,2017-11-16.
[31] GB 23200.13—2016.食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.
[32] 王翔,宋国新,胡耀铭.GC/MS研究茶叶中拟除虫菊酯类农药残留的提取方法[J].质谱学报,2008,29(2):97-100.WANG Xiang,SONG Guoxin,HU Yaoming.Study on extaction of pyrethroid pesticide multi-residues in tea by GC/MS[J].Journal of Chinese Mass Spectrometry Society,2008,29(2):97-100(in Chinese).
[33] AOAC Official Method 2007.01.Pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate[EB/OL].http://www.weber.hu/Downloads/SPE/QuEChERS/AOAC_2007_01.pdf.
[34] 庞国芳,范春林,李岩,康健,常巧英,卜明楠,金春丽,陈辉.茶叶中653种农药化学品残留GC-MS、GC-MS/MS与LC-MS/MS分析方法:国际AOAC方法评价预研究[J].分析测试学报,2012,31(9):1 017-1 030.PANG Guofang,FAN Chunlin,LI Yan,KANG Jian,CHANG Qiaoying,PU Mingnan,JIN Chunli,CHEN Hui.Determination of 653 pesticides and chemical contaminants residues in tea by GC-MS,GC-MS/MS and LC-MS/MS:the pre-collaborative study of aoac method efficiency evaluation[J].Journal of Instrumental Analysis,2012,31(9):1 017-1 030(in Chinese).
[35] SN/T 1950—2007.进出口茶叶中多种有机磷农药残留量的检测方法气相色谱法[S].北京:中国标准出版社,2007.