高效液相色谱-串联质谱法同时测定贝类中22种农药残留

引用本文: 范广宇, 唐秀, 张云青, 孟祥龙, 梁振纲. 高效液相色谱-串联质谱法同时测定贝类中22种农药残留[J]. 色谱, 2019, 37(6): 612-618. doi: 10.3724/SP.J.1123.2018.12026 shu

Citation: FAN Guangyu, TANG Xiu, ZHANG Yunqing, MENG Xianglong, LIANG Zhengang. Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(6): 612-618. doi: 10.3724/SP.J.1123.2018.12026 shu

高效液相色谱-串联质谱法同时测定贝类中22种农药残留

1.
连云港海关, 江苏连云港 222042;
2.
海南出入境检验检疫局技术中心, 海南海口 570311
基金项目:
南京海关科技计划项目（2017KJ12）；海关总署应急保障计划（2018IK048）.

摘要: 建立了高效液相色谱-三重四极杆质谱（HPLC-MS/MS）同时测定贝类中22种农药残留的分析方法。样品经含0.1%（v/v）甲酸的乙腈提取，N-丙基乙二胺（PSA）和石墨化碳黑（GCB）净化，然后采用ACE UltraCore 2.5 SuperC18柱（100 mm×2.1 mm，2.5 μm）分离，以甲醇-0.1%（v/v）甲酸水溶液为流动相梯度洗脱，流速为0.4 mL/min，柱温为35 ℃，然后以电喷雾电离（ESI）源，在多反应监测（MRM）、正离子模式下，采用三重四极杆质谱检测。22种农药在各自的线性范围内线性关系良好，相关系数均大于0.997，检出限为0.1~0.3 μg/kg，定量限为0.3~1.0 μg/kg。在3个添加水平下，22种农药的平均回收率为65.2%~109.4%，相对标准偏差为1.3%~15.2%（n=6）。该方法操作简单，快速，准确度高，灵敏度高，可用于贝类中22种农药残留的同时检测。

关键词:

English

Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry

1.
Lianyungang Customs, Lianyungang 222042, China;
2.
Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau, Haikou 570311, China
Received Date: 17 December 2018
Fund Project:
Science and Technology Plan Project of Nanjing Customs (No. 2017KJ12)

Abstract: A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1% (v/v) formic acid in acetonitrile, cleaned up with primary secondary amine (PSA) and graphitized carbon black (GCB), and then separated on an ACE UltraCore 2.5 Super C18 column (100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1% (v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients (r²) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2% (n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.

Key words:

high-performance liquid chromatography (HPLC)
/ triple quadrupole mass spectrometry (MS/MS)
/ pesticide residues
/ shellfish

1. [1] Sousa J C G, Ribeiro A R, Barbosa M O, et al. J Hazard Mater, 2018, 344:146
2. [2] Papadakis E N, Tsaboula A, Kotopoulou A, et al. Sci Total Environ, 2015, 536(3):793
3. [3] Shen F, Xu Y J, Song T, et al. Chinese Journal of Chromatography, 2018, 36(10):1018 沈斐, 许燕娟, 宋挺, 等. 色谱, 2018, 36(10):1018
4. [4] Tankiewicz M, Biziuk M. Anal Bioanal Chem, 2018, 410(5):1533
5. [5] Cao F F, Fei J Y, Xu R J, et al. China Measurement & Test, 2017, 43(3):53 曹方方, 费金岩, 许人骥, 等. 中国测试, 2017, 43(3):53
6. [6] Zhong Z, Guo Y M, Liu Q. Journal of Anhui Agricultural Sciences, 2015, 43(23):119 钟志, 郭远明, 刘琴. 安徽农业科学, 2015, 43(23):119
7. [7] Sun X M, Hu H M, Zhong Z, et al. J Sep Sci, 2015, 38(4):626
8. [8] Fu J W, Huang Z J, Chen M J, et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2018, 54(9):1015 符靖雯, 黄子敬, 陈孟君, 等. 理化检验-化学分册, 2018, 54(9):1015
9. [9] Fu L, Lu X B, Tan J, et al. J Environ Sci, 2018, 63(1):116
10. [10] Li L, Dong W F, Liu M Y, et al. China Food Additives, 2017(7):188 李莉, 董伟峰, 刘梦遥, 等. 中国食品添加剂, 2017(7):188
11. [11] Zhang H W, Liu H H, Tian X H, et al. Journal of Chinese Mass Spectrometry Society, 2015, 36(2):177 张华威, 刘慧慧, 田秀慧, 等. 质谱学报, 2015, 36(2):177
12. [12] Huang W, Zhang J J, Liu H, et al. Journal of Food Safety & Quality, 2016, 7(2):746 黄武, 章晶晶, 刘辉, 等. 食品安全质量检测学报, 2016, 7(2):746
13. [13] Cho H R, Park J S, Kim J, et al. Anal Bioanal Chem, 2015, 407(30):9043
14. [14] Lazartigues A, Wiest L, Baudot R, et al. Anal Bioanal Chem, 2011, 400(7):2185
15. [15] Wang X C, Shu B, Li S, et al. Talanta, 2017, 162:90
16. [16] Liu H H, Zhang H W, Wei X, et al. Chinese Journal of Analytical Chemistry, 2018, 46(3):386 刘慧慧, 张华威, 魏潇, 等. 分析化学, 2018, 46(3):386
17. [17] Wang Y J, Huang H L, Dong C Z, et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2013, 49(4):398 王玉健, 黄惠玲, 董存柱, 等. 理化检验-化学分册, 2013, 49(4):398
18. [18] Rahman M M, Abd El-Aty A M, Kim S W, et al. J Sep Sci, 2017, 40 (1):203
19. [19] Wang L Z, Huang X Y, Wang D F, et al. Chinese Journal of Chromatography, 2015, 33(5):501 王连珠, 黄小燕, 王登飞, 等. 色谱, 2015, 33(5):501
20. [20] GB 2763-2016

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱-串联质谱法同时测定贝类中22种农药残留

English

Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry

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中国化学会秘书处

高效液相色谱-串联质谱法同时测定贝类中22种农药残留

English

Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry

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