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

引用本文: 张新忠, 罗逢健, 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): 1686-1692. doi: 10.3724/SP.J.1096.2012.20093 shu

Citation: ZHANG Xin-Zhong, LUO Feng-Jian, ZHANG Fen, LIU Guang-Ming, LOU Zheng-Yun, CHEN Zong-Mao. 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): 1686-1692. doi: 10.3724/SP.J.1096.2012.20093 shu

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

通讯作者: 陈宗懋

基金项目:
本文系国家茶叶产业技术体系建设专项资金资助项目(No.CARS-23) (No.CARS-23)

中国农业科学院基本科研业务费专项(No.0032012026) (No.0032012026)

农业部农药残留标准制(修)订CAC标准转化项目资助 (修)

摘要: 建立了分散固相萃取净化、气相色谱串联质谱法(GC-MS/MS)测定茶叶、芒果和西葫芦中噻螨酮和噻嗪酮残留分析方法, 并对噻螨酮、噻嗪酮的质谱裂解规律和基质效应进行了分析。噻嗪酮和噻螨酮分别在0.040-4.0 mg/L和0.025-2.5 mg/L浓度范围内呈线性关系, 相关系数0.9910, 检出限分别为0.005和0.010 mg/L;不同样品中噻螨酮和噻嗪酮平均回收率为83.6%-116.9%之间, 相对标准偏差为2.0%-15.7%, 方法定量限为茶叶中0.010 mg/kg, 西葫芦、芒果中为0.002 mg/kg采用此方法抽检我国不同地区市场上的120份芒果、西葫芦样品, 均未检出噻螨酮噻嗪酮残留;检测20份噻嗪酮田间残留试验茶叶样, 均未检出噻嗪酮残留(低于3.9 mg/kg)。

关键词:

English

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

1.
¹ Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China;

Corresponding author: 陈宗懋

Received Date: 08 February 2012
Fund Project:
本文系国家茶叶产业技术体系建设专项资金资助项目(No.CARS-23)

中国农业科学院基本科研业务费专项(No.0032012026)

农业部农药残留标准制(修)订CAC标准转化项目资助

Abstract: A novel and sensitive method was developed and validated for the simultaneous determination of hexythiazox and buprofezin residue in tea, mango and marrow using gas chromatography coupled with tandem mass spectrometry. Target compounds were extracted by acetonitrile followed by dispersive solid phase extraction cleanup. The fragmentation pathway and matrix effect were investigated. Over the concentration in the range of 0.040-4.000 mg/L for buprofezin and 0.025-2.5 mg/L for hexythiazox in different matrix, the correlation coefficients (r) of the calibration curves were above 0.9910, and the limits of detection (LODs) were 0.005 mg/L and 0.010 mg/L for each other. The average recoveries of hexythiazox and buprofezin in different matrix at three spiked concentration levels ranged from 83.6% to 116.9% with relative standard deviations (RSDs) between 2.0% and 15.7% (n=5). The limits of quantitation (LOQs) of hexythiazox and buprofezin, were 0.010 mg/kg in green tea and 0.002 mg/kg in marrow and mango sample. Then, the proposed method was successfully applied to the routine market monitoring of mango and marrow in different regions in China, there was no hexythiazox and buprofezin residue detected in the all of samples (n=120); and it has also been applied to the residue analysis of buprofezin field test samples (n=20) in tea garden, the residues of buprofezin were from not detected to 3.9 mg/kg.

Key words:

Dispersive solid phase extraction
/ Gas chromatography tandem mass spectrometry
/ Tea
/ Mango
/ Marrow
/ Hexythiazox
/ Buprofezin

1. [1]
  1 ZHOU Chun-Mei, LI Qing. Agriculture & Technology, 2001, 21(5): 36-391 ZHOU Chun-Mei, LI Qing. Agriculture & Technology, 2001, 21(5): 36-39
2. [2]
  周春梅, 李青. 农业与技术, 2001, 21(5): 36-39周春梅, 李青. 农业与技术, 2001, 21(5): 36-39
3. [3]
  2 ZHU Liang-Tian. Pesticide. Beijing: Chemical Industry Press, 2004: 183, 2062 ZHU Liang-Tian. Pesticide. Beijing: Chemical Industry Press, 2004: 183, 206
4. [4]
  朱良天. 农药. 北京: 化学工业出版社, 2004: 183, 206朱良天. 农药. 北京: 化学工业出版社, 2004: 183, 206
5. [5]
  3 http://www.m5.ws001.squarestart.ne.jp/foundation/search.html3 http://www.m5.ws001.squarestart.ne.jp/foundation/search.html
6. [6]
  4 http://db.foodmate.net/pesticide/index.php4 http://db.foodmate.net/pesticide/index.php
7. [7]
  5 http://ec.europa.eu/sanco_pesticides/public/index.cfm5 http://ec.europa.eu/sanco_pesticides/public/index.cfm
8. [8]
  6 DING Li-Ping, WEI Yun-Hao. Agrochemicals, 2011, 50(5): 352-3556 DING Li-Ping, WEI Yun-Hao. Agrochemicals, 2011, 50(5): 352-355
9. [9]
  丁立平, 魏云昊. 农药, 2011, 50(5): 352-355丁立平, 魏云昊. 农药, 2011, 50(5): 352-355
10. [10]
  7 ZHANG Shui-Ba, YI Jun, YE Jiang-Lei, ZHENG Wen-Hui, CAI Xue-Qin, GONG Zhen-Bin. Chinese J. Chromatogr., 2004, 22(2): 154-1577 ZHANG Shui-Ba, YI Jun, YE Jiang-Lei, ZHENG Wen-Hui, CAI Xue-Qin, GONG Zhen-Bin. Chinese J. Chromatogr., 2004, 22(2): 154-157
11. [11]
  张水坝, 易军, 叶江雷, 郑文慧, 蔡学勤,弓振斌. 色谱, 2004, 22(2): 154-157张水坝, 易军, 叶江雷, 郑文慧, 蔡学勤,弓振斌. 色谱, 2004, 22(2): 154-157
12. [12]
  8 Łozowicka B, Jankowska M, Kaczyński P. Food Control, 2012, 25(2): 561-5758 Łozowicka B, Jankowska M, Kaczyński P. Food Control, 2012, 25(2): 561-575
13. [13]
  9 Determination of Hexythiazox Residues in Pome and Citrousfruits. National Standards of the People's Republic of China. GB/T 5009.173-20039 Determination of Hexythiazox Residues in Pome and Citrousfruits. National Standards of the People's Republic of China. GB/T 5009.173-2003
14. [14]
  梨果类、柑桔类水果中噻螨酮残留量的测定. 中华人民共和国国家标准. GB/T 5009.173-2003梨果类、柑桔类水果中噻螨酮残留量的测定. 中华人民共和国国家标准. GB/T 5009.173-2003
15. [15]
  10 DONG Jing, GONG Xiao-Ming, ZHANG Li, WANG Hong-Tao. Chinese J. Anal. Lab., 2008, 27(3): 91-9410 DONG Jing, GONG Xiao-Ming, ZHANG Li, WANG Hong-Tao. Chinese J. Anal. Lab., 2008, 27(3): 91-94
16. [16]
  董静, 宫小明, 张立, 王洪涛. 分析试验室, 2008, 27(3): 91-94董静, 宫小明, 张立, 王洪涛. 分析试验室, 2008, 27(3): 91-94
17. [17]
  11 Ravelo-Pérez L M, Hernández-Borges J, Asensio-Ramos M, Rodríguez-Delgado M . J. Chromatogr. A, 2009, 1216(43): 7336-734511 Ravelo-Pérez L M, Hernández-Borges J, Asensio-Ramos M, Rodríguez-Delgado M . J. Chromatogr. A, 2009, 1216(43): 7336-7345
18. [18]
  12 ZHU Tao, ZHOU Hong-Chen, YAN Qiu-Cheng, WANG Yong, TIAN Xiao-Lin. Chinese J. Anal. Lab., 2007, 26(10): 72-7512 ZHU Tao, ZHOU Hong-Chen, YAN Qiu-Cheng, WANG Yong, TIAN Xiao-Lin. Chinese J. Anal. Lab., 2007, 26(10): 72-75
19. [19]
  朱涛, 周宏琛, 闫秋成, 王勇, 田晓林. 分析试验室, 2007, 26(10): 72-75朱涛, 周宏琛, 闫秋成, 王勇, 田晓林. 分析试验室, 2007, 26(10): 72-75
20. [20]
  13 LI Yong-Jun, HUANG Zhi-Qiang, DAI Hua, ZHANG Ying. J. Instrum. Anal., 2002, 21(2): 78-8013 LI Yong-Jun, HUANG Zhi-Qiang, DAI Hua, ZHANG Ying. J. Instrum. Anal., 2002, 21(2): 78-80
21. [21]
  李拥军, 黄志强, 戴华, 张莹. 分析测试学报, 2002, 21(2): 78-80李拥军, 黄志强, 戴华, 张莹. 分析测试学报, 2002, 21(2): 78-80
22. [22]
  14 Lesueur C, Knittl P, Gartner M, Mentler A, Fuerhacker M. Food Control, 2008, 19(9): 906-91414 Lesueur C, Knittl P, Gartner M, Mentler A, Fuerhacker M. Food Control, 2008, 19(9): 906-914
23. [23]
  15 Didier O, Patrick E, Claude C. Anal. Chim. Acta, 2004, 520(1-2): 33-4515 Didier O, Patrick E, Claude C. Anal. Chim. Acta, 2004, 520(1-2): 33-45
24. [24]
  16 Ondrej L, Jana U, Jan P, Jana H. J. Chromatogr. A, 2010, 1217(5): 648-65916 Ondrej L, Jana U, Jan P, Jana H. J. Chromatogr. A, 2010, 1217(5): 648-659
25. [25]
  17 Bienvenida G L, Juan F G R, Ana L, Amadeo R F A, Antonio M D. J. Chromatogr. A, 2010, 1217(39): 6022-603517 Bienvenida G L, Juan F G R, Ana L, Amadeo R F A, Antonio M D. J. Chromatogr. A, 2010, 1217(39): 6022-6035
26. [26]
  18 GB/T 19648-2006. Determination of 500 Pesticides and Related Chemicals Residues in Fruits and Vegetables——GC-MS Method. National Standards of the People's Republic of China.18 GB/T 19648-2006. Determination of 500 Pesticides and Related Chemicals Residues in Fruits and Vegetables——GC-MS Method. National Standards of the People's Republic of China.
27. [27]
  水果和蔬菜中500种农药及相关化学品残留的测定——气相色谱-质谱法. 中华人民共和国国家标准. GB/T 19648-2006水果和蔬菜中500种农药及相关化学品残留的测定——气相色谱-质谱法. 中华人民共和国国家标准. GB/T 19648-2006
28. [28]
  19 GB/T 20769-2008. Determination of 450 Pesticides and Related Chemicals Residues in Fruits and Vegetables——LC-MS-MS Method. National Standards of the People's Republic of China.19 GB/T 20769-2008. Determination of 450 Pesticides and Related Chemicals Residues in Fruits and Vegetables——LC-MS-MS Method. National Standards of the People's Republic of China.
29. [29]
  水果和蔬菜中450种农药及相关化学品残留量的测定——液相色谱-串联质谱法. 中华人民共和国国家标准. GB/T 20769-2008水果和蔬菜中450种农药及相关化学品残留量的测定——液相色谱-串联质谱法. 中华人民共和国国家标准. GB/T 20769-2008
30. [30]
  20 GB/T 23204-2008. Determination of 519 Pesticides and Related Chemicals Residues in Tea——GC-MS Method. National Standards of the People's Republic of China.20 GB/T 23204-2008. Determination of 519 Pesticides and Related Chemicals Residues in Tea——GC-MS Method. National Standards of the People's Republic of China.
31. [31]
  茶叶中519种农药及相关化学品残留量的测定——气相色谱-质谱法. 中华人民共和国国家标准. GB/T 23204-2008茶叶中519种农药及相关化学品残留量的测定——气相色谱-质谱法. 中华人民共和国国家标准. GB/T 23204-2008
32. [32]
  21 GB/T 23205-2008. Determination of 448 Pesticides and Related Chemicals Residues in Tea——LC-MS-MS Method. National Standards of the People's Republic of China.21 GB/T 23205-2008. Determination of 448 Pesticides and Related Chemicals Residues in Tea——LC-MS-MS Method. National Standards of the People's Republic of China.
33. [33]
  茶叶中448种农药及相关化学品残留量的测定——液相色谱-串联质谱法. 中华人民共和国国家标准. GB/T 23205-2008茶叶中448种农药及相关化学品残留量的测定——液相色谱-串联质谱法. 中华人民共和国国家标准. GB/T 23205-2008
34. [34]
  22 ZHANG Xin-Zhong, LUO Feng-Jian, LIU Guang-Ming, LOU Zheng-Yun, CHEN Zong-Mao. Chinese J. Anal. Chem., 2011, 39(9): 1329-133522 ZHANG Xin-Zhong, LUO Feng-Jian, LIU Guang-Ming, LOU Zheng-Yun, CHEN Zong-Mao. Chinese J. Anal. Chem., 2011, 39(9): 1329-1335
35. [35]
  张新忠, 罗逢健, 刘光明, 楼正云, 陈宗懋. 分析化学, 2011, 39(9): 1329-1335张新忠, 罗逢健, 刘光明, 楼正云, 陈宗懋. 分析化学, 2011, 39(9): 1329-1335
36. [36]
  23 QIAN Peng-Cheng, CHEN Jun-Zhi, CHEN Fan. Fine Chemicals, 2011, 28(3): 300-30223 QIAN Peng-Cheng, CHEN Jun-Zhi, CHEN Fan. Fine Chemicals, 2011, 28(3): 300-302
37. [37]
  钱鹏程, 陈均志, 陈帆. 精细化工, 2011, 28(3): 300-302钱鹏程, 陈均志, 陈帆. 精细化工, 2011, 28(3): 300-302
38. [38]
  24 Inspection and Quarantine of the People's Republic of China. Residues Analysis Quality Control Guide. Beijing, 200224 Inspection and Quarantine of the People's Republic of China. Residues Analysis Quality Control Guide. Beijing, 2002
39. [39]
  中国人民共和国质量监督检验检疫总局. 残留分析质量控制指南. 北京, 2002中国人民共和国质量监督检验检疫总局. 残留分析质量控制指南. 北京, 2002

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 431
HTML全文浏览量: 33

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

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

通讯作者: 陈宗懋

English

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

Corresponding author: 陈宗懋

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

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

通讯作者: 陈宗懋

English

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

Corresponding author: 陈宗懋

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