高效液相色谱-串联质谱法测定水产品中镇静剂及其代谢物残留

引用本文: 张璇, 杨光昕, 孔聪, 翟文磊, 冯华锋, 沈晓盛, 于慧娟. 高效液相色谱-串联质谱法测定水产品中镇静剂及其代谢物残留[J]. 分析化学, 2021, 49(3): 460-467. doi: 10.19756/j.issn.0253-3820.201531 shu

Citation: ZHANG Xuan, YANG Guang-Xin, KONG Cong, ZHAI Wen-Lei, FENG Hua-Feng, SHEN Xiao-Sheng, YU Hui-Juan. Determination of Tranquilizer and Their Metabolites Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(3): 460-467. doi: 10.19756/j.issn.0253-3820.201531 shu

高效液相色谱-串联质谱法测定水产品中镇静剂及其代谢物残留

张璇 ^1, ,
杨光昕 ^1, ,
孔聪 ^{1,
,} ,
翟文磊 ^2, ,
冯华锋 ^3, ,
沈晓盛 ^1, ,
于慧娟 ^1,

1.
中国水产科学研究院东海水产研究所, 农业农村部水产品质量安全控制重点实验室(上海), 上海 200090;
2.
北京市农业质量标准与技术研究中心, 北京 100097;
3.
上海商学院, 酒店管理学院食品科学系, 上海 200235

通讯作者: 孔聪,E-mail:kongcong@gmail.com

基金项目:
农业行业标准修制订项目（Nos.SCB-20021，SCB-20025）、上海市农业委员会项目（Nos.沪农科推字（2016）第1-4-1号，2020-02-08-00-07-F01464）、上海市法医学重点实验室课题项目（司法鉴定科学研究院，No.KF1910）和国家自然科学基金项目（No.31701698）资助。

摘要: 建立了液相色谱-串联三重四极杆质谱（HPLC-MS/MS）法测定水产品中镇静剂及其代谢物共12种化合物残留量的方法。样品加入地西泮-d₅、安眠酮-d₇、氯丙嗪-d₆内标，加入200 μL 1 mol/L NaOH溶液后，采用乙酸乙酯进行提取，氮吹浓缩，用80%乙腈溶解，PSA和C₁₈分散固相萃取材料进行净化，内标法进行定量分析。以2 mmol/L乙酸铵-0.1%甲酸和甲醇为流动相，以Capcell PAK C₁₈ MGⅡ色谱柱（100 mm×2.0 mm，5 μm）进行分离，在质谱多反应监测模式（MRM）下测定。本方法在0.5~20 μg/kg范围内线性相关系数（R²）均大于0.999，方法检出限为0.5 μg/kg，定量限为1.0 μg/kg，在14种水产品中添加水平为1、5和10 μg/kg时的回收率在80.6%~119.4%之间，相对标准偏差（RSD）在0.05%~14.5%之间。对2020年8月份采自上海的167个鱼、虾、蟹、贝等实际样品筛查发现，4.79%的水产品中检出地西泮，含量范围介于检出限与定量限之间。本方法简单快捷、准确度高、灵敏度高，适用于不同种类水产品中镇静剂类药物的检测。

关键词:

English

Determination of Tranquilizer and Their Metabolites Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
Key Laboratory of Control of Quality and Safety for Aquatic Products (Shanghai), Ministry of Agriculture and Rural Affairs, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai 200090, China;
2.
(Beijing Research Center for Agricultural Standards and Testing, Beijing 100097, China;
3.
Department of Food Science, College of Hospitality Management, Shanghai Business School, Shanghai 200235, China

Corresponding author: KONG Cong, kongcong@gmail.com

Received Date: 01 September 2020
Revised Date: 18 December 2020
Fund Project:
Standard Project of Ministry of Agriculture and Rural Affairs, China (Nos. SCB-20021, SCB-20025), the Shanghai Agriculture Applied Technology Development Program (Nos. T2016010401, 2020-02-08-00-07-F01464), the Shanghai Key Laboratory of Forensic Medicine (Academy of Forensic Science, No.KF1910), and the National Natural Science Foundation of China (No.31701698).

Abstract: A method for determination of tranquilizer and their metabolites residues in aquatic products by HPLC-MS/MS was developed. The samples were added with internal standard of diazepam-d₅, methaqualone-d₇ and chlorpromazine-d₆, and then extracted by ethyl acetate under alkaline conditions. Then the extract was dried under nitrogen, and the residues were dissolved in 80% acetonitrile solution and cleaned up with PSA and C₁₈. Isotope internal standard was used for quantification. The analytes were separated by a Capcell PAK C₁₈ MGⅡ(100 mm×2.0 mm, 5 μm) column, and gradient eluted with a mixed solution of (2 mmol/L ammonium acetate+0.1% formic acid) and methanol. The mass spectrometric analysis was carried out under multiple reaction monitoring mode. Good linearity of the calibration curves was obtained in the concentration range of 0.5-20.0 μg/kg with the correlation coefficients (R²) of more than 0.999. The limit of detection for this method was 0.5 μg/kg and the quantitative limit was 1.0 μg/kg. The average recoveries at three fortified levels (1, 5 and 10 μg/kg) were 80.6%-119.4%, and the RSDs ranged from 0.05% to 14.5%. This method was simple, rapid with high accuracy and sensitivity, and was suitable for detection of tranquilizer residues in aquatic products.

Key words:

High performance liquid chromatography-tandem mass spectrometry
/ Tranquilizer
/ Aquatic products
/ Diazepam
/ Chlorpromazine

1. [1]
  XIE Jing, CAO Jie. J. Shanghai Ocean Univ., 2020, kns.cnki.net/kcms/detail/31.2024.S.20200609.0959.002.html. 谢晶, 曹杰. 上海海洋大学学报, 2020, kns.cnki.net/kcms/detail/31.2024.S.20200609.0959.002.html.
2. [2]
  ZOU You, SHAO Lin-Zhi, CHEN Si-Min, OUYANG Shao-Lun, LIN Feng. Chin. J. Chromatogr., 2017, 35(8):801-807. 邹游, 邵琳智, 陈思敏, 欧阳少伦, 林峰. 色谱, 2017, 35(8):801-807.
3. [3]
  LI Yuan, HUANG Bao-Sheng, ZHANG Chang-Feng. Food Ind., 2019, 40(12):251-255. 李元, 黄宝生, 张长峰. 食品工业, 2019, 40(12):251-255.
4. [4]
  Ministry of Agriculture and Rural Affairs. No. 250, List of Drugs and Other Compounds Prohibited in Food Animals. Bulletin of the Ministry of Agriculture of the People's Republic of China. 食品动物中禁止使用的药品及其他化合物清单. 中华人民共和国农业农村部公告第250号.
5. [5]
  GB 31650-2019. National Food Safety Standard Maximum Residue Limits for Veterinary Drugs in Foods. National Standards of the People's Republic of China. 食品安全国家标准食品中兽药最大残留限量. 中华人民共和国国家标准. GB 31650-2019.
6. [6]
  Codex Alimentarius Commission (CAC). Codex Alimentarius Commission Maximum Residue Limits for Veterinary Drugs in Foods Updated as at the 35th Session of the Codex Alimentarius Commission (July 2012).
7. [7]
  European Parliament and Council. Regulation (EC) No. 470/2009 of the European Parliament and the Council. 2009.
8. [8]
  WANG J, WANG Y L, PAN Y H, CHEN D M, LIU Z L, FENG L, PENG D P, YUAN Z H. Food Chem., 2017, 221:1004-1013.
9. [9]
  PENG C F, DUAN X, SONG S, XUE F. Int. J. Mol. Sci., 2013, 14(10):19474-19483.
10. [10]
  SRIVASTAVA V. Pharmacophore, 2016, 7:63-73.
11. [11]
  SOLTANINEJAD K, KARIMI M, NATEGHI A, DARAEI B. Iran. J. Pharm. Res., 2016, 15(2):457.
12. [12]
  XU F M, LI Q, WEI W L, LIU L Y, LI H B. Chromatographia, 2018, 81(12):1695-1703.
13. [13]
  HAN L, ZHU J Y, FAN X, ZHANG C, TU K, PENG J, WANG J H, PAN L Q. Sensors, 2020, 20(16):4441.
14. [14]
  LIANG X, FENG T T, WU J H, DU M, QIN L, WANG Z Y, XU X B. Food Anal. Methods, 2017, 11:790-796.
15. [15]
  LI Rong, YANG Lu-Qi, ZHANG Peng-Yun, LUO Yang-Dan, ZHANG Peng-Jie, GAO Yong-Qing. Chin. J. Chromatogr., 2018, 36(2):125-135. 李蓉, 杨璐齐, 张鹏云, 罗阳丹, 张朋杰, 高永清. 色谱, 2018, 36(2):125-135.
16. [16]
  WANG Y X, PENG D P, ZHU Y F, XIE S Y, PAN Y H, CHEN D M, TAO Y F, YUAN Z H. J. Sep. Sci., 2019, 42(10):1915-1929.
17. [17]
  WEI J M, LUO Y Z, ZHANG L. J. Sci. Food Agric., 2015, 95(3):598-606.
18. [18]
  LEE S, HAN E, IN S, CHOI H, CHUNG H, CHUNG K H. J. Anal. Toxicol., 2011, 35(5):312- 315.
19. [19]
  MADRY M M, SPYCHER B S, KUPPER J, FUERST A, BAUMGARTNER M R, KRAEMER T, NAEGELI H. BMC Vet. Res., 2016, 12:84-94.
20. [20]
  LIU Jia-Yang, HUANG Xu, JIA Hong-Xin. J. Instrum. Anal., 2017, 36(3):305-311. 刘家阳, 黄旭, 贾宏新. 分析测试学报, 2017, 36(3):305-311.
21. [21]
  LI Zhi-Gang, LI Hui-Chen, MA Yan-Hong, WANG Shou-Wei, REN Nan, GUO Wen-Ping, GUO Chao, LI Ying-Ying. Food Sci., 2019, 40(24):320-324. 李志刚, 李慧晨, 马燕红, 王守伟, 任南, 郭文萍, 郭超, 李莹莹. 食品科学, 2019, 40(24):320-324.
22. [22]
  HU Hai-Shan, ZHANG Yun-Wei, ZHAO Shu-E, LU Hui. J. Food Safe. Food Qual., 2018, 9(20):5319-5323. 胡海山, 张云伟, 赵淑娥, 芦慧. 食品安全质量检测学报, 2018, 9(20):5319-5323.
23. [23]
  YU Hui-Juan, QIAN Bei-Lei, HUANG Dong-Mei, SU Hui, GU Run-Run, FENG Bing. Chin. Fish. Qual. Stand., 2011, 1(1):54-59. 于慧娟, 钱蓓蕾, 黄冬梅, 苏慧, 顾润润, 冯兵. 中国渔业质量与标准, 2011, 1(1):54-59.
24. [24]
  WANG Shou-Ying, KONG Cong, YANG Guang-Xin, YU Hui-Juan. Qual. Saf. Agro-prod., 2020, 3:31-35. 王守英, 孔聪, 杨光昕, 于慧娟. 农产品质量与安全, 2020, 3:31-35.
25. [25]
  ZHAO Qiao-Ling, ZHANG Wei-Ying, TANG Hai-Feng, WANG Ping-Ya, DAI Yi-Fei, JIANG Ling-Bo. Food Sci. Technol., 2019, 44(12):335-341. 赵巧灵, 张薇英, 汤海凤, 王萍亚, 戴意飞, 蒋玲波. 食品科技, 2019, 44(12):335-341.
26. [26]
  PAOLONI A, SOLFRIZZO M, BIBI R, PECORCLLI I. J. Environ. Sci. Health B, 2018, 53(5):327-333.
27. [27]
  HUANG Y S, LI C, HU H Y, WANG Y T, SHEN M Y, NIE S P, CHEN J, ZENG M M, XIE M Y. J. Agric. Food Chem., 2019, 67:5017-5025.
28. [28]
  XU Zhi-Yi, CHEN Meng-Ting, HOU Xi-Ai, LIU Dan. Chin. J. Anal. Chem., 2020, 48(7):928-936. 徐芷怡, 陈梦婷, 侯锡爱, 刘丹. 分析化学, 2020, 48(7):928-936.
29. [29]
  SU You-Zhi, LI Fang, ZHAO Guang-Yao, HUANG Zhi-Qiang, LEI Hong-Qin, LI Yan-Mei. Chin. J. Anal. Chem., 2017, 45(1):118-123. 粟有志, 李芳, 赵光跃, 黄志强, 雷红琴, 李艳美. 分析化学, 2017, 45(1):118-123.
30. [30]
  WANG Si-Wei, LIU Yan-Ping, SUN Hai-Bin. Chin. J. Anal. Chem., 2018, 46(5):704-709. 王思威, 刘艳萍, 孙海滨. 分析化学, 2018, 46(5):704-709.
31. [31]
  CHEN Jie-Feng, LIANG Ming, XIAN Yan-Ping, WU Yu-Luan, WEN Shao-Kai, WANG Bin, WANG Li, HOU Xiang-Chang, LIU Dong-Hong. Chin. J. Anal. Chem., 2019, 47(8):1258-1266. 陈杰锋, 梁明, 冼燕萍, 吴玉銮, 温少楷, 王斌, 王莉, 侯向昶, 刘冬虹. 分析化学, 2019, 47(8):1258-1266.
32. [32]
  MATUSZEWSKI B K, CONSTANZER M L, CHAVEZ-ENG C M. Anal. Chem., 2003, 75(13):3019-3030.
33. [33]
  GB/T 20763-2006. Method for Determination of Acetopromaizine, Chlorpromazine, Haloperidol, Propionylpromazine, Xylazine, Azaperol and Carazolol Residues in Porcine Kidney and Muscle Tissues-LC-MS-MS Method. National Standards of the People's Republic of China. 猪肾和肌肉组织中乙酰丙嗪、氯丙嗪、氟哌啶醇、丙酰二甲氨基丙吩噻嗪、甲苯噻嗪、阿扎哌隆、阿扎哌醇、咔唑心安残留量的测定. 中华人民共和国国家标准. GB/T 20763-2006.
34. [34]
  GB 29697-2013. Determination of Diazepam and Methaqualone Residues in Animal Derived Food-Gas Chromatography-Mass Spectrometry. National Standards of the People's Republic of China. 动物性食品中地西泮和安眠酮多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 29697-2013.
35. [35]
  GB/T 27404-2008. Criterion on Quality Control of Laboratories-Chemical Testing of Food. National Standards of the People's Republic of China. 实验室质量控制规范食品理化检测. 中华人民共和国国家标准. GB/T 27404-2008.

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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-串联质谱法测定水产品中镇静剂及其代谢物残留

通讯作者: 孔聪,E-mail:kongcong@gmail.com

English

Determination of Tranquilizer and Their Metabolites Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: KONG Cong, kongcong@gmail.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱-串联质谱法测定水产品中镇静剂及其代谢物残留

通讯作者: 孔聪,E-mail:kongcong@gmail.com

English

Determination of Tranquilizer and Their Metabolites Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: KONG Cong, kongcong@gmail.com

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？

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