液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物

引用本文: 梁秀美, 王祥云, 薛晓锋, 齐沛沛, 刘真真, 刘之炜, 周莉, 王新全, 王强. 液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物[J]. 分析化学, 2017, 45(4): 553-559. doi: 10.11895/j.issn.0253-3820.160833 shu

Citation: LIANG Xiu-Mei, WANG Xiang-Yun, XUE Xiao-Feng, QI Pei-Pei, LIU Zhen-Zhen, LIU Zhi-Wei, ZHOU Li, WANG Xin-Quan, WANG Qiang. Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(4): 553-559. doi: 10.11895/j.issn.0253-3820.160833 shu

液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物

梁秀美 ^1,2, ,
王祥云 ^1,3, ,
薛晓锋 ^4, ,
齐沛沛 ^1, ,
刘真真 ^1, ,
刘之炜 ^1, ,
周莉 ^1, ,
王新全 ^1, ,
王强 ^1,

1.
省部共建国家重点实验室培育基地"浙江省植物有害生物防控重点实验室", 农业部农药残留检测重点实验室, 浙江省农业科学院农产品质量标准研究所, 杭州 310021;
2.
南京农业大学植物保护学院, 南京 210095;
3.
中国农业大学理学院, 北京 100094;
4.
中国农业科学院蜜蜂研究所, 北京 100093
基金项目:
本文系浙江省自然基金项目（No.LQ14B070004）、特色农产品全产业链安全风险管控项目（No.ZJNY2016001）和蜂产品全产业链安全风险管控项目（No.ZJNY2016001-02）资助

摘要: 建立了蜂蜜和蜂花粉中吡虫啉及其代谢物吡虫啉烯烃、吡虫啉脲、6-氯烟酸的液相色谱-串联质谱（LC-MS/MS）检测方法。在QuEChERS方法基础上，针对目标物化学性质和样品杂质情况，对提取溶液的pH值、提取次数、净化材料等参数进行了优化。最终以5%甲酸-乙腈溶液提取两次，无水MgSO₄、NaCl盐析分层，提取液经增强型脂类去除材料（EMR）净化，以LC-MS/MS进行测定，基质外标法进行定量分析。结果表明，蜂蜜和蜂花粉中吡虫啉、吡虫啉烯烃、吡虫啉脲、6-氯烟酸的平均加标回收率为86.0%~111.5%，相对标准偏差在1.7%~9.6%之间，检出限分别为0.20、3.50、0.40和14.00 μg/kg，定量限分别为0.60、11.64、1.20和45.00 μg/kg。本方法分析速度快、灵敏度高、重现性好，适用于蜂蜜和蜂花粉中吡虫啉及其3种代谢物的快速测定。

关键词:

English

Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry

1.
State Key Lab Breeding Base for Zhejiang Sustainable Plant Pest Control, Ministry of Agriculture, Key Lab for Pesticide Residue Detection, Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China;
2.
College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China;
3.
College of Science, China Agricultural University, Beijing 100094, China;
4.
Institute of Apiculture Research, Chinese Academy of Agricultural Sciences, Beijing 100093, China
Received Date: 15 November 2016
Revised Date: 06 February 2017

Abstract: A method was developed for the determination of imidacloprid and its metabolites imidacloprid olefin, imidacloprid urea and 6-chloronicotinic acid in honey and bee pollen by liquid chromatography tandem mass spectrometry (LC-MS/MS). On the basis of typical QuEChERS method, the pH and times of extraction solvent, sorbents were optimized to ensure the extraction efficiency and the purification of extraction. Finally, the method was developed as follows: matrix was extracted with 5% formic acid-acetonitrile twice, and the extraction was cleaned with enhanced matrix removal-lipid (EMR), detected with LC-MS/MS and quantified with external matrix standards. The results indicated that the average spiked recoveries of imidacloprid, imidacloprid olefin, imidacloprid urea and 6-chloronicotinic acid in honey and pollen samples were 86.0%-111.5% with relative standard deviations (RSDs) of 1.7%-9.6%, the LODs were 0.20, 3.50, 0.40 and 14.00 μg/kg, and the LOQs were 0.60, 11.64, 1.20 and 45.00 μg/kg. The method was rapid and simple with high sensitivity and good reproducibility, and suitable for the determination of imidacloprid and its three metabolites residues in honey and bee pollen.

Key words:

Liquid chromatography tandem mass spectrometry
/ Honey
/ Hollen
/ Imidacloprid
/ Imidacloprid olefin
/ Imidacloprid urea
/ 6-Chloronicotinic acid
/ Enhanced matrix removal-Lipid

1. [1]
  WEI Li-Na, YE Fei. Pestic. Sci. Adm., 2013, 34(5): 27-34 魏立娜, 叶非. 农药科学与管理, 2013, 34(5): 27-34
2. [2]
  WANG Xiao-Hui, WAN Xiao-Chun, HOU Ru-Yan. Journal of Tea Science, 2012, 32(3): 203-209 王孝辉, 宛晓春, 侯如燕. 茶叶科学, 2012, 32(3): 203-209
3. [3]
  ZHAO YI-Nan, GAO Jing-Lin, WANG Yu-Jie, LIU Jun-Feng, ZHAO Dong-Xiang. Agrochemicals, 2014, 53(3): 206-209 赵怡楠, 高景林, 王玉洁, 刘俊峰, 赵冬香. 农药, 2014, 53(3): 206-209
4. [4]
  Decourtye A, Armengaud C, Renou M, Devillers J, Cluzeau S, Gauthier M, Pham-Delegue M H. Pestic. Biochem. Physiol., 2004, 78(2): 83-92
5. [5]
  ZHANG Heng-Min, ZHAO Ping, YAN Qiu-Xu, LI Xin. Agrochemicals, 2012, 51(12): 858-862 张恒敏, 赵平, 严秋旭, 李新. 农药, 2012, 51(12): 858-862
6. [6]
  Cresswell J E. Ecotoxicology, 2011, 20(1): 149-157
7. [7]
  Whitehorn P R, O'Connor S, Wackers F L, Goulson D. Science, 2012, 336(6079): 351-352
8. [8]
  LIN Zhe-Guang, MENG Fei, ZHENG Huo-Qing, ZHOU Ting, HU Fu-Liang. Acta Entomol. Sin., 2014, 57(5): 607-615 蔺哲广, 孟飞, 郑火青, 周婷, 胡福良. 昆虫学报, 2014, 57(5): 607-615
9. [9]
  Suchail S, Guez D, Belzunces L P. Environ. Toxicol. Chem., 2001, 20(11): 2482-2486
10. [10]
  LAN Shan-Shan, LIU Hong-Cheng, LI Qi-Wan, SHAO Jin-Liang, YANG Fang. J. Anal. Sci., 2011, 27(2): 171-174 兰珊珊, 刘宏程, 黎其万, 邵金良, 杨芳. 分析科学学报, 2011, 27(2): 171-174
11. [11]
  YANG Dong-Dong, CONG Lu-Jing, TIAN Ming-Ming, WANG Ming-Hua. Chinese J. Anal.Chem., 2014, 42(6): 872-877 杨东冬, 丛路静, 田明明, 王鸣华. 分析化学, 2014, 42(6): 872-877
12. [12]
  Fidente P, Seccia S, Vanni F, Morrica P. J. Chromatogr. A, 2005, 1094(1-2): 175-178
13. [13]
  Martel A C, Lair C. Inter. J. Environ. Anal. Chem., 2011, 91(10): 978-988
14. [14]
  Kamel A. J. Agric. Food Chem., 2010, 58(10): 5926-5931
15. [15]
  Garcia M D G, Galera M M, Valverde R S, Galanti A, Girotti S. J. Chromatogr. A, 2007, 1147(1): 17-23
16. [16]
  Anastassiades M, Lehotay S J, Stajnbaher D, Schenck F J. J. AOAC Int., 2003, 86(2): 412-431
17. [17]
  Wiesta L, Bulete A, Giroud B, Fratta C, Amic S, Lambert O, Pouliquen H, Arnaudguilhem C. J. Chromatogr. A, 2011, 1218(34): 5743-5756
18. [18]
  Li Y, Kelley R A, Anderson T D, Lydy M J. Talanta, 2015, 140: 81-87
19. [19]
  Han L J, Matarrita J, Sapozhnikova Y, Lehotay S J. J. Chromatogr. A, 2016, 1449: 17-29
20. [20]
  SONG Shu-Ling, LI Chong-Jiu, MA Xiao-Dong, RAO Zhu, WEI Qian. Chinese J. Anal. Chem., 2008, 36(11): 1526-1530 宋淑玲, 李重九, 马晓东, 饶竹, 韦倩. 分析化学, 2008, 36(11): 1526-1530
21. [21]
  Nardic D, Bonellif. Rapid. Commun. Mass Spectrom., 2006, 20(18): 2709-2716

扫一扫看文章

计量

PDF下载量: 25
文章访问数: 1196
HTML全文浏览量: 113

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物

English

Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物

English

Determination of Imidacloprid and Its Three Metabolites in Honey and Bee Pollen by Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs