[1]张乐,赵文文,廖锦林,等.基于QuEChERS-HPLC-MS方法的夏大豆中嗪草酮残留研究[J].大豆科学,2021,40(03):403-411.[doi:10.11861/j.issn.1000-9841.2021.03.0403]
　ZHANG Le,ZHAO Wen-wen,LIAO Jin-lin,et al.Study on Residue of Metribuzin in Summer Soybean Based on QuEChERS-HPLC-MS[J].Soybean Science,2021,40(03):403-411.[doi:10.11861/j.issn.1000-9841.2021.03.0403]
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基于QuEChERS-HPLC-MS方法的夏大豆中嗪草酮残留研究

《大豆科学》[ISSN:1000-9841/CN:23-1227/S] 卷: 第40卷 期数: 2021年03期 页码: 403-411 栏目: 出版日期: 2021-05-20
Title:
Study on Residue of Metribuzin in Summer Soybean Based on QuEChERS-HPLC-MS
作者:
张乐1; 赵文文2; 廖锦林3; 郭静远1; 邵华1; 佘永新1; 金芬1; 王静1
(1.中国农业科学院 农业质量标准与检测技术研究所，北京 100081； 2.海南大学 林学院，海南 海口 570228； 3.中央社会主义学院，北京 100081)
Author(s):
ZHANG Le1;  ZHAO Wen-wen2;  LIAO Jin-lin3;  GUO Jing-yuan1;  SHAO Hua1;  SHE Yong-xin1;  JIN Fen1;  WANG Jing1
(1.Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China; 2.College of Forestry, Hainan University, Haikou 570228, China; 3.The Central Institute of Socialism, Beijing 100081, China)
关键词:
嗪草酮; 夏大豆; QuEChERS; 高效液相色谱-串联质谱法; 稳定性
Keywords:
Metribuzin;  Summer soybean;  QuEChERS;  HPLC-MS;  Stability
DOI:
10.11861/j.issn.1000-9841.2021.03.0403
文献标志码:
A
摘要:
为高效分析嗪草酮在夏大豆青豆（带荚）、青豆秸秆、大豆、大豆秸秆中的残留安全性，本研究建立了QuEChERS样品前处理-高效液相色谱串联质谱法，评价70%嗪草酮水分散粒剂在夏大豆上一年六地残留的安全性。夏大豆青豆（带荚）、青豆秸秆、大豆、大豆秸秆经QuEChERS前处理技术同步实现乙腈提取，PSA和C18净化，再经质谱多反应监测模式扫描，基质匹配标准曲线外标法定量。结果显示：嗪草酮浓度在0.01~0.20 mg?L-1时具有良好的线性关系（r=0.999 7），0.01，0.05和0.20 mg?kg-1加标浓度下，嗪草酮在青豆（带荚）、青豆秸秆、大豆、大豆秸秆中的平均回收率为96.3% ~101.7%，相对标准偏差为1.1%~5.2%，定量下限为 0.01 mg?kg-1。该检测方法简单、快速、灵敏度及准确度高，能够满足夏大豆中嗪草酮残留量的检测要求。对青豆（带荚）、青豆秸秆、大豆、大豆秸秆中的最终残留量进行分析，残留量均小于0.010 mg?kg-1，均低于我国规定的大豆中嗪草酮的MRL值0.05 mg?kg-1。
Abstract:
In order to effectively analyze the residue safety of metribuzin in summer soybean(with pod) , green bean straw, soybean and soybean straw, this study established a QuEChERS sample pretreatment coupled with High Performance Liquid Chromatography-tandem Mass Spectrometry (HPLC-MS), to evaluate the residual safety of 70% metribuzin water dispersible granule in summer soybeans sampled from six areas in one year. The extraction of metribuzin from summer soybean green beans(with pod), green bean straw, soybean and soybean straw were extracted by QuEChERS pretreatment technology with acetonitrile, purified by PSA and C18 simultaneously, then scanned by MS spectrometry multi-reaction monitoring mode, and quantified by matrix matching standard curve external standard method. Metribuzin in 0.01-0.20 mg?L-1 range has a good linear relationship, the correlation coefficient was 0.999 7, the standard addition concentrations were 0.01, 0.05 and 0.20 mg?kg-1 , the average recovery of metribuzin in green bean (with pod), green beans straw, soybean and soybean straw was 96.3%-101.7%, the relation standard deviation (RSD) was 1.1%-5.2%, and the quantitative limit was 0.01 mg?kg-1. This method is simple, rapid, sensitive and accurate, meeting to the requirement of detecting the residual quantity of metribuzin in summer soybean. The final residues of 70% metribuzin water dispersible granule in green beans(with pod), green beans straw, soybean and soybean straw were all less than 0.010 mg?kg-1, which were lower than the MRL value of 0.05 mg?kg-1 metribuzin in soybean stipulated by China.

参考文献/References:

［1］Wauchope R D, Buttler T M, Hornsby A G, et al. The SCS/ARS/CES pesticide properties database for environmental decision-making［J］.Reviews of Environmental Contamination and Toxicology, 1992, 123(1): 1-155.［2］中华人民共和国卫生部.食品安全国家标准食品中农药最大残留限量: GB 2763-2019［S］. 北京:中国标准出版社, 2019: 198. (Ministry of Health of the PRC. Maximum Residue Limits for Pesticides in Food: GB 2763-2019［S］. Beijing: Standards Press of China, 2019: 198).［3］胡继业, 刘丰茂, 潘灿平. 嗪草酮的高效液相色谱分析［J］. 莱阳农学院学报, 1998, 15(4): 272- 273. (Hu J Y, Liu F M, Pan C P. Determination of metribuzin by HPLC［J］. Journal of Laiyang Agricultural College, 1998, 15(4): 272- 273.) ［4］杨俊柱. 70％嗪草酮可湿性粉剂的反相高效液相色谱测定［J］.安徽化工, 2008, 34(6): 57-59. (Yang J Z. Determination of 70% metribuzin WP by RP-HPLC［J］. Anhui Chemical Industry, 2008, 34(6): 57-59.)［5］亓晓莉. QuEChERS-高效液相色谱-串联质谱法快速检测玉米及土壤中嗪草酮残留［J］. 广东化工, 2015, 42(12): 195-196. (Qi X L. Rapid and simultaneous determination of metribuzin in maize and soil by QuEChERS and HPLC-MS/MS［J］. Guangdong Chemical Industry, 2015,42(12):195-196.)［6］梁林, 任玉鹏, 李文平, 等. 嗪草酮在马铃薯和土壤中的残留分析方法及消解动［J］. 农药, 2017, 12(16): 908-911. (Liang L, Ren Y P, Li W P, et al. Dissipation dynamics and residue analysis of metribuzin in potato and soil［J］. Agrochemicals, 2017, 12(16): 908-911.)［7］陈春红, 逯忠斌, 侯志广. 嗪草酮在土壤和大豆中的残留动态研究［J］. 江苏农业科学, 2011(1): 332- 335. (Chen C H, Lu Z B, Hou Z G. Residue dynamics of metribuzin in soil and soybean［J］. Jiangsu Agricultural Science, 2011(1): 332- 335.)［8］Hu J, Deng Z, Liu C, et al. Simultaneous analysis of herbicide metribuzin and quizalofop-p-ethyl residues in potato and soil by GC-ECD［J］. Chromatographia, 2010, 72(7-8): 701-706.［9］张小玲, 谢艳丽, 张宇, 等. 气-质联用法检测番茄中的嗪草酮及其主要代谢产物［J］. 食品科技, 2015, 40(10): 252-255. (Zhang X L, Xie Y L, Zhang Y, et al. Determination of metribuzin and its major metabolites by gas chromatography-mass spectrometry［J］. Food Science and Technology, 2015, 40(10): 252-255.)［10］刘伟, 吴文君. 气-质联机对嗪草酮原药及其主要杂质的分析［J］. 农药, 2006, 45(9): 614-617. (Liu W, Wu W J. GC-MS analysis of metribuzin technical and its main impurities［J］. Agrochemicals, 2006, 45(9): 614-617.)［11］谢丽琪, 蓝芳, 林黎, 等. 气相色谱-质谱法同时测定粮谷及油籽中多种酰胺类除草剂残留量［J］. 分析测试学报, 2007(3): 365-367, 372. (Xie L Q, Lan F, Lin L, et al. Simultaneous determination of multiple acetanilide herbicide residues in cereals and oil seeds by gas chromatography-mass spectrometry［J］. Journal of Instrumental Analysis, 2007(3): 365-367, 372.)［12］Anastassiades M, Lehotay S J, tajnbaher D, et al. 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.［13］Caldas S S, Bolzan C M, Cerqueira M B, et al. Evaluation of a modified QuEChERS extraction of multiple classes of pesticides from a rice paddy soil by LC-APCI-MS/MS［J］. Journal of Agricultural and Food Chemistry, 2011, 59(22): 11918-11926.［14］Wilkowska A, Biziuk M.Determination of pesticide residues in food matrices using the QuEChERS Methodology［J］. Food Chemistry, 2011, 125(3): 803-812.［15］Dong F S, Chen X, Liu X G,et al. Simultaneous determination of five pyrazole fungicides in cereals, vegetables and fruits using liquid chromatography/tandem mass spectrometry［J］. Journal of Chromatography A, 2012, 1262: 98-106.［16］张丹华, 陈芳, 王垚垚, 等. QuEChERS-毛细管电泳法测定紫薯中的农药残留［J］. 商丘师范学院学报, 2015(9): 46-50. (Zhang D H, Chen F, Wang Y Y, et al. Determination of pesticides in purple potato using QuEChERS combined with capillary electrophoresis［J］.Journal of Shangqiu Normal University, 2015(9): 46-50.)［17］陈国峰, 李雪茹, 刘峰, 等. 82%嗪〖DK1〗?异丙甲〖DK1〗?滴辛酯乳油在大豆上残留的检测方法及膳食风险评估［J］. 大豆科学, 2020, 39(5): 781-789. (Chen G F, Li X R, Liu F, et al. Detection methods of 82% metolachlor〖DK1〗?metribuzin〖DK1〗?2，4-D-Ethylhexyl EC on soybean and its dietary risk assessment［J］. Soybean Science, 2020, 39(5): 781-789.)［18］中华人民共和国农业部.农作物中农药残留试验准则: NY/T 788-2018［S］. 北京: 中华人民共和国农业部, 2018: 2-3. (Ministry of Agriculture of the People’s Republic of China. Criteria for testing pesticide residues in crops: NY/T 788-2018［S］. Beijing: Ministry of Agriculture of the People’s Republic of China, 2018: 2-3.)［19］Environmental Protection Agency Office of Pesticide Programs. Reregistration eligibility decision (RED) metribuzin［EB/OL］. US EPA Archive Document, 1998: 24.［20］European Food Safety Authority. Modification of the existing maximum residue level for metribuzin in olives for oil production［R］. EFSA Journal, 2016, 14(10): 4591.［21］宋淑荣, 张玉婷, 郭永泽, 等. 嗪草酮70%可湿性粉剂在大豆上残留动态研究［J］. 天津农业科学, 2010, 16(5): 94-96. (Song S R, Zhang Y T, Guo Y Z, et al. Residue dynamics of metribuzin 70% WP in soybean and soil［J］. Tianjin Agricultural Sciences, 2010, 16(5): 94-96.)［22］中华人民共和国农业部.农作物中农药残留试验准则: NY/T 788-2004［S］. 北京:中华人民共和国农业部, 2004. (Ministry of Agriculture of the People’s Republic of China. Criteria for testing pesticide residues in crops: NY/T 788-2004［S］. Beijing: Ministry of Agriculture of the People’s Republic of China, 2004.)

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备注/Memo

收稿日期：2021-01-12

基金项目：国家重点研发计划（2019YFC1605601）。
第一作者：张乐（1998—），女，在读硕士，主要从事食品加工与安全研究。E-mail:nkyzhangle@163.com。
通讯作者：邵华（1977—），女，硕士，副研究员，主要从事农药残留与检测技术研究。E-mail:nkshaohua@163.com。

更新日期/Last Update: 2021-07-20