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

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

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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;
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(Beijing Research Center for Agricultural Standards and Testing, Beijing 100097, China;
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Department of Food Science, College of Hospitality Management, Shanghai Business School, Shanghai 200235, China

Corresponding author: KONG Cong, kongcong@gmail.com
Received Date: 1 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).

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