同位素稀释-液相色谱-串联质谱法同时测定养殖水体中23种镇静剂

张秋云; 杨洪生; 朱晓华; 霍春林; 谭秀慧; 陈慧敏

引用本文:	张秋云,杨洪生,朱晓华,霍春林,谭秀慧,陈慧敏.同位素稀释-液相色谱-串联质谱法同时测定养殖水体中23种镇静剂[J].环境监控与预警,2024,16(2):46-52
	ZHANG Qiuyun,YANG Hongsheng,ZHU Xiaohua,HUO Chunlin,TAN Xiuhui,CHEN Huimin.Simultaneous Determination of 23 Sedative Residues in Aquaculture Water by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2024,16(2):46-52

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同位素稀释-液相色谱-串联质谱法同时测定养殖水体中23种镇静剂
张秋云^1,2，杨洪生^1,2*，朱晓华^1,2，霍春林¹，谭秀慧^1,2，陈慧敏³
1. 江苏省淡水水产研究所，江苏南京 210017；2. 江苏省水产质量检测中心，江苏南京 210017；3. 上海爱博才思分析仪器贸易有限公司，上海 200335

摘要:

建立了同位素稀释-液相色谱-串联质谱法（LC-MS/MS）同时测定养殖水体中23种镇静剂残留的方法。样品经0.45 μm滤膜过滤后，用Oasis HLB固相萃取柱净化，浓缩后用50%的甲醇水定容。以1%甲酸水溶液和乙腈为流动相，采用Agilent InfiniityLab Poroshell 120 SB-C18色谱柱分离后，在多反应监测模式下测定，内标法定量。结果表明，23种镇静剂在0.5～100ng/L质量浓度范围内线性关系良好（r>0.99），检出限和定量限分别为0.1~0.3和0.4 ~1.0 ng/L。加标回收率为73.5%~117.6%，相对标准偏差（RSD）为1.1%~9.9%。该方法前处理简单，净化效果较好，灵敏度较高，适用于池塘养殖水体中23种镇静剂类药物残留的快速检测。

关键词: 同位素稀释液相色谱-串联质谱池塘养殖水体镇静剂

DOI：DOI：10.3969/j.issn.1674-6732.2024.02.007

分类号:X832

基金项目:江苏现代农业产业技术体系建设项目（JATS［2021］368）；江苏省“333工程”培养资金资助项目（BRA2020374）；蓝色粮仓科技创新重点专项（2020YFD0900300）

Simultaneous Determination of 23 Sedative Residues in Aquaculture Water by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry

ZHANG Qiuyun^1,2， YANG Hongsheng^1,2*， ZHU Xiaohua^1,2， HUO Chunlin¹， TAN Xiuhui^1,2， CHEN Huimin³

1. Freshwater Fishery Research Institute of Jiangsu Province， Nanjing， Jiangsu 210017， China； 2.Aquatic Product Quality Inspection Center of Jiangsu Province， Nanjing， Jiangsu 210017， China； 3.Shanghai AB Sciex Analytical Instrument Trading Co. Ltd.， Shanghai 200335， China

Abstract:

A method for simultaneous determination of 23 sedative residues in aquaculture water by isotope dilution liquid chromatography tandem mass spectrometry(LC-MS/MS) was established. The samples were filtered by 0.45 μm filter membrane， purified by solid phase extraction column(Oasis HLB column)， then concentrated the eluate and brought to volume with 50% methanol 50% water. By using 1% formic acid aqueous solution and acetonitrile as mobile phase， the targets were separated by an Agilent InfinityLab Poroshell 120 SB-C18 chromatographic column， and determined in multi reaction monitoring mode and quantified by internal standard method. The results showed that the linearity of 28 sedatives was good in the concentration range of 0.5～100 ng/L (r > 0.99)， and the detection limits and quantitative limits were 0.1～0.3 and 0.4～1.0 ng/L， respectively. The average recovery was 73.5%～117.6% and the relative standard deviations(RSD) were 1.1%～ 9.9%. This method has simple pretreatment， good purification effect and high sensitivity. It can be used for the rapid detection of 23 sedative drug residues in pond aquaculture water.

Key words: Isotope dilution Liquid chromatography tandem mass spectrometry Pond aquaculture water body Sedative