加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留

引用本文: 焦慧泽, 陆世清, 侯迪, 张前前. 加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留[J]. 色谱, 2019, 37(6): 605-611. doi: 10.3724/SP.J.1123.2019.01011 shu

Citation: JIAO Huize, LU Shiqing, HOU Di, ZHANG Qianqian. Determination of pyrethroid pesticides in tea by accelerated solvent extraction and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(6): 605-611. doi: 10.3724/SP.J.1123.2019.01011 shu

加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留

1.
钦州海关国家燕窝及营养保健品监测重点实验室(钦州), 广西钦州 535000;
2.
中国海洋大学化学化工学院, 山东青岛 266100

摘要: 建立了加速溶剂萃取（ASE）-超高效液相色谱（UPLC）-串联质谱法（MS/MS）测定茶叶中拟除虫菊酯类农药残留的方法。ASE萃取温度为80 ℃，萃取压力为10.34 MPa，以正己烷-丙酮（2∶1，v/v）为溶剂静态萃取5 min，循环一次。萃取液浓缩后经GCB/NH₂-Florisil柱净化，UPLC分离，MS/MS正离子扫描（ESI⁺）、多反应离子监测（MRM）模式进行分析，外标法定量。线性回归分析表明：10种拟除虫菊酯的浓度与其峰面积的线性关系显著，相关系数（r）均不小于0.9995，检出限（LOD）在0.5~5.0 μg/kg之间，定量限（LOQ）在1.6~16.6 μg/kg之间；在定量限、0.4 mg/kg以及最高残留限量（MRL，无MRL的加入1 mg/kg）3个水平进行添加回收试验（n=7），回收率为68.7%~103.8%，RSD为0.8%~13.2%。该方法前处理简单，耗时短，灵敏度和准确度高，可满足茶叶中痕量拟除虫菊酯类农药残留测定的要求。

关键词:

English

Determination of pyrethroid pesticides in tea by accelerated solvent extraction and ultra-performance liquid chromatography-tandem mass spectrometry

1.
State Key Testing Laboratory of Edible Bird's Nest and Nutritional Health Food(Qinzhou), Qinzhou Customs, Qinzhou 535000, China;
2.
College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266100, China
Received Date: 14 January 2019

Abstract: A method was developed for the determination of pyrethroid pesticides in tea by accelerated solvent extraction (ASE) combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted from tea using n-hexane and acetone (2:1, v/v) for 5 min at 10.34 MPa and 80℃ via a single cycle of accelerated solvent extraction. The extract was purified by GCB/NH₂ and Florisil columns, analyzed by UPLC-MS/MS in positive electrospray ionization (ESI⁺) and multiple reaction monitoring (MRM) modes, and quantified by the external standard method. Regression analysis revealed that the linear relationships between mass concentration and peak area are significant for the 10 pyrethroid pesticides, and the correlation coefficients (r) are all not less than 0.9995. The limits of detection (LOD) of the 10 pyrethroid pesticides ranged from 0.5 μg/kg to 5.0 μg/kg and the limits of quantification (LOQ) ranged from 1.6 μg/kg to 16.6 μg/kg. The recoveries of all the pesticides ranged from 68.7% to 103.8% at the spiked levels of LOQ, 0.4 mg/kg and maximum residue limit (MRL) (added 1 mg/kg without MRL) with RSDs ranging from 0.8% to 13.2% (n=7). The proposed method is simple, rapid, sensitive, and accurate, and could be effective for trace analysis of pyrethroid pesticides in tea.

Key words:

ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
/ accelerated solvent extraction (ASE)
/ pyrethroid
/ tea

1. [1] Zhao L N, Lai Z N, Li X L, et al. Ecology and Environmental Sciences, 2013, 22(8):1408 赵李娜, 赖子尼, 李秀丽, 等. 生态环境学报, 2013, 22(8):1408
2. [2] Xie J P, Huang Q T, Liu J, et al. Chinese Journal of Health Laboratory Technology, 2016, 26(9):1229 谢俊平, 黄秋婷, 刘君, 等. 中国卫生检验杂志, 2016, 26(9):1229
3. [3] Ren R, Wang S T, He H L, et al. Chinese Journal of Health Laboratory Technology, 2016, 26(11):1645 任韧, 王姝婷, 何华丽, 等. 中国卫生检验杂志, 2016, 26(11):1645
4. [4] Shukla Y, Arora A, Singh A. Toxicology, 2001, 163:1
5. [5] Neelima P, Rao K G, Rao G S, et al. Int J Biol Med Res, 2016, 7(2):5574
6. [6] Domingues V, Cabral M, Alves A, et al. Anal Lett, 2009, 42(4):706
7. [7] Sun P, Gao Y L, Wang J M, et al. Chinese Journal of Pesticide Science, 2016, 18(4):497 孙鹏, 高玉玲, 王金梅, 等. 农药学学报, 2016, 18(4):497
8. [8] Tripathy V, Saha A, Patel D J, et al. J Environ Sci Health, Part B, 2016, 51(8):508
9. [9] Chen B, Wu F Q, Wu W D, et al. Microchem J, 2016, 126:415
10. [10] Niu Z, Yu C, He X, et al. J Pharm Biomed Anal, 2017, 143:222
11. [11] Liu L, Zhang Q, Wang H Y, et al. Chinese Journal of Chromatography, 2017, 35(8):860 刘丽, 张琦, 王海雁, 等. 色谱, 2017, 35(8):860
12. [12] Qu L, Li Y, Zeng J, et al. Chinese Journal of Chromatography, 2017, 35(7):778 曲栗, 李优, 曾静, 等. 色谱, 2017, 35(7):778
13. [13] Huang W, Li N, Xu R H, et al. Chinese Journal of Chromatography, 2018, 36(12):1303 黄微, 李娜, 徐瑞晗, 等. 色谱, 2018, 36(12):1303
14. [14] Fan W, Tang F, Yue Y D. Chinese Agricultural Science Bulletin, 2010, 26(3):238 樊玮, 汤锋, 岳永德. 中国农学通报, 2010, 26(3):238
15. [15] Yu L, Dong L L. Journal of Analytical Science, 2016, 32(2):218 于玲, 董丽丽. 分析科学学报, 2016, 32(2):218
16. [16] Xing H, Hou D F, Hou C Q, et al. Agrochemicals, 2017, 56(7):492 邢红, 侯德粉, 侯春青, 等. 农药, 2017, 56(7):492
17. [17] Yang L, Wen Y Y, Gong Z B. Chinese Journal of Analytical Chemistry, 2010, 38(7):968 杨琳, 温裕云, 弓振斌. 分析化学, 2010, 38(7):968
18. [18] Liu Q, Sun L, Zhang L. Journal of Instrumental Analysis, 2010, 29(10):1048 刘琪, 孙雷, 张骊. 分析测试学报, 2010, 29(10):1048
19. [19] Shao H Y, Xu G, Wu M H, et al. Chinese Journal of Analytical Chemistry, 2013, 41(9):1315 邵海洋, 徐刚, 吴明红, 等. 分析化学, 2013, 41(9):1315
20. [20] Chu N M, Meng X, Kang Y Q, et al. Food Science, 2016, 37(24):239 褚能明, 孟霞, 康月琼, 等. 食品科学, 2016, 37(24):239
21. [21] Deng M L, Chen J C, Duan Y P, et al. Chinese Journal of Analysis Laboratory, 2014, 33(3):351 邓美林, 陈俊赤, 段云鹏, 等. 分析试验室, 2014, 33(3):351
22. [22] Lu X L, Ye M J, Zhou W L. Agrochemicals, 2014, 53(11):825 陆小磊, 叶美君, 周卫龙. 农药, 2014, 53(11):825
23. [23] GB 2763-2016

扫一扫看文章

计量

PDF下载量: 4
文章访问数: 424
HTML全文浏览量: 23

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

加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留

English

Determination of pyrethroid pesticides in tea by accelerated solvent extraction and ultra-performance 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

加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留

English

Determination of pyrethroid pesticides in tea by accelerated solvent extraction and ultra-performance 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