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

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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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