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  

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

作　　者：张璇[1] 杨光昕 孔聪[1] 翟文磊 冯华锋 沈晓盛[1] 于慧娟[1] ZHANG Xuan;YANG Guang-Xin;KONG Cong;ZHAI Wen-Lei;FENG Hua-Feng;SHEN Xiao-Sheng;YU Hui-Juan(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;Beijing Research Center for Agricultural Standards and Testing,Beijing 100097,China;Department of Food Science,College of Hospitality Management,Shanghai Business School,Shanghai 200235,China)

机构地区：[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

出　　处：《分析化学》2021年第3期460-467,I0001-I0003,共11页Chinese Journal of Analytical Chemistry

基　　金：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);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-d_(5)、安眠酮-d_(7)、氯丙嗪-d_(6)内标,加入200μL 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C_(18)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 C_(18)MGⅡ色谱柱(100 mm×2.0 mm,5μm)进行分离,在质谱多反应监测模式(MRM)下测定。本方法在0.5~20μg/kg范围内线性相关系数(R^(2))均大于0.999,方法检出限为0.5μg/kg,定量限为1.0μg/kg,在14种水产品中添加水平为1、5和10μg/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。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-d_(5),methaqualone-d_(7)and chlorpromazine-d_(6),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 C_(18).Isotope internal standard was used for quantification.The analytes were separated by a Capcell PAK C 18 MGⅡ(100 mm×2.0 mm,5μm)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 0.5-20.0μg/kg with the correlation coefficients(R^(2))of more than 0.999.The limit of detection for this method was 0.5μg/kg and the quantitative limit was 1.0μg/kg.The average recoveries at three fortified levels(1,5 and 10μg/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.

关 键 词：液相色谱-串联质谱 镇静剂 水产品 地西泮 氯丙嗪 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]