分散液相微萃取荧光法测定果蔬中残留吡蚜酮
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摘要
[目的]利用分散液相微萃取和表面活性剂增敏,建立果蔬中吡蚜酮残留量的荧光分光光度快速测定法。[方法]用二氯甲烷作为萃取剂,丙酮作为分散剂对样品进行前处理。以水作溶剂,320μL十二烷基硫酸钠(SDS)(0.1 mol/L)作增敏剂,室温静置10 min。1 cm石英比色皿作吸收池,于激发波长(λ_(ex))312 nm、发射波长(λ_(em))349 nm处测定荧光强度。[结果]在0.02~1.00 mg/L范围内,吡蚜酮浓度与荧光强度线性关系良好,检出限为0.0196 mg/kg。加标回收率为87.73%~99.06%,RSD为2.93%~9.67%。[结论]新建方法可用于水果蔬菜中吡蚜酮残留测定。
[Aims] A rapid method for determination of pymetrozine residues in fruits and vegetables by fluorescence spectrophotometry combined with dispersive liquid-liquid microextraction was established. [Methods] The samples were pretreated with dichloromethane as the extractant and acetone as the dispersant. Then, water was used as solvent,320 μL of sodium dodecyl sulfate(SDS)(0.1 mol/L) was added in solution as sensitizer. The sample solution was kept at room temperature for 10 minutes. Quartz cuvette(1 cm) was used as absorption cell. The fluorometric analysis of the sample was performed at the excitation wavelength( λ_(ex)) of 312 nm and the emission wavelength(λ_(em)) of 349 nm.[Results] The linear correlation coefficient of the calibration curve was 0.9965 when the concentration was 0.02-1.00 mg/L. The limit of detection was 0.0196 mg/kg. The recovery rate was 87.73-99.06% with the relative standard deviation of 2.93-9.67%. [Conclusions] The method can be used to determine the pymetrozine residues in fruits and vegetables.
[Aims] A rapid method for determination of pymetrozine residues in fruits and vegetables by fluorescence spectrophotometry combined with dispersive liquid-liquid microextraction was established. [Methods] The samples were pretreated with dichloromethane as the extractant and acetone as the dispersant. Then, water was used as solvent,320 μL of sodium dodecyl sulfate(SDS)(0.1 mol/L) was added in solution as sensitizer. The sample solution was kept at room temperature for 10 minutes. Quartz cuvette(1 cm) was used as absorption cell. The fluorometric analysis of the sample was performed at the excitation wavelength( λ_(ex)) of 312 nm and the emission wavelength(λ_(em)) of 349 nm.[Results] The linear correlation coefficient of the calibration curve was 0.9965 when the concentration was 0.02-1.00 mg/L. The limit of detection was 0.0196 mg/kg. The recovery rate was 87.73-99.06% with the relative standard deviation of 2.93-9.67%. [Conclusions] The method can be used to determine the pymetrozine residues in fruits and vegetables.
引文
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[9]王全胜,曹梦超,刘雅楠,等.Qu ECh ERS结合UPLC-ESIMS/MS分析吡蚜酮和异丙威SC在稻田中的残留特征[J].农业环境科学学报,2015,34(3):431-437.
[10]唐俊,曾凯,张敏,等.基于Qu ECh ERS-液质联用法同时测定大米中五种新型农药残留[J].食品工业,2016,7(3):276-279.
[11]冯义志,潘金菊,刘伟.超高效液相色谱质谱联用检测小麦中吡蚜酮的残留分析方法[J].农药,2015,54(1):48-50.
[12]MERCAN H,YILMAZ E,INAM R.Determination of Insecticide Pymetrozine by Differential Pulse Polaroraphy/Application to Lake Water and Orange Juice[J].Journal of Hazardous Materials,2007,141(3):700-706.
[13]许金钩,王尊本.荧光分析法[M].3版.北京:科学出版社,2006:317-318.
[14]夏鑫鑫,吕勇智,韩笑,等.分散液相微萃取技术在农药残留分析中的应用[J].农药,2016,55(3):160-165.
[15]赵燕燕,耿成光,白洁,等.胶束增敏同步荧光-双波长法同时测定血浆中儿茶酚胺类神经递质[J].河北大学学报(自然科学版),2010,30(3):264-270.
[16]陕西出入境检验检疫局.2010B132.进出口食品中吡蚜酮残留量的测定液相色谱-质谱/质谱法编制说明[DB/OL].(2010-10-22)Http://www.doc88.com/p-9377127773458.html.
[2]杨辉,陈力华,任凤莲,等.高效液相色谱法测定水稻中吡蚜酮残留量[J].农药,2010,49(11):825-827.
[3]JANG J,RAHMAN M M,KO A Y,et al.A Matrix Sensitive Gas Chromatography Method for the Analysis of Pymetrozine in Red Pepper:Application to Dissipation Pattern and PHRL[J].Food Chemistry,2014,146:448-454.
[4]段婷婷,郑永权.超高效液相色谱法测定吡蚜酮在棉花和土壤中的残留[J].农药学学报,2011,13(5):547-550.
[5]GUAN Wen-bi,LI Zhuo-nan,ZHANG Hong-yan,et al.Amine Modified Graphene as Reversed Dispersive Solid Phase Extraction Materials Combined with Liquid Chromatography Tandem Mass Spectrometry for Pesticide Multi-residue Analysis in Oil Crops[J].Journal of Chromatography A,2013,1286:1-8.
[6]LEE S W,CHOI J H,CHO S K,et al.Development of a New Qu ECh ERS Method Based on Dry Ice for the Determination of 168 Pesticides in Paprika Using Tandem Mass Spectrometry[J].Journal of Chromatography A,2011,1218:4366-4377.
[7]许秀莹,施海燕,王鸣华,等.气相色谱-质谱联用测定大米中6种烟碱类农药残留[J].质谱学报,2012(2):99-103.
[8]沈燕,刘贤进,徐敦明,等.LC-MS-MS法检测小麦粉中12种农药的残留[J].农药,2011,50(11):831-833.
[9]王全胜,曹梦超,刘雅楠,等.Qu ECh ERS结合UPLC-ESIMS/MS分析吡蚜酮和异丙威SC在稻田中的残留特征[J].农业环境科学学报,2015,34(3):431-437.
[10]唐俊,曾凯,张敏,等.基于Qu ECh ERS-液质联用法同时测定大米中五种新型农药残留[J].食品工业,2016,7(3):276-279.
[11]冯义志,潘金菊,刘伟.超高效液相色谱质谱联用检测小麦中吡蚜酮的残留分析方法[J].农药,2015,54(1):48-50.
[12]MERCAN H,YILMAZ E,INAM R.Determination of Insecticide Pymetrozine by Differential Pulse Polaroraphy/Application to Lake Water and Orange Juice[J].Journal of Hazardous Materials,2007,141(3):700-706.
[13]许金钩,王尊本.荧光分析法[M].3版.北京:科学出版社,2006:317-318.
[14]夏鑫鑫,吕勇智,韩笑,等.分散液相微萃取技术在农药残留分析中的应用[J].农药,2016,55(3):160-165.
[15]赵燕燕,耿成光,白洁,等.胶束增敏同步荧光-双波长法同时测定血浆中儿茶酚胺类神经递质[J].河北大学学报(自然科学版),2010,30(3):264-270.
[16]陕西出入境检验检疫局.2010B132.进出口食品中吡蚜酮残留量的测定液相色谱-质谱/质谱法编制说明[DB/OL].(2010-10-22)Http://www.doc88.com/p-9377127773458.html.