Simultaneous Determination of Ten Tranquilizers and Their Metabolites in Aquatic Products by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

WANG Xu-feng; WANG Qiang; ZHANG Ying-xia; HUANG Ke

doi:10.19969/j.fxcsxb.23040604

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Simultaneous Determination of Ten Tranquilizers and Their Metabolites in Aquatic Products by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-07-12

- Simultaneous Determination of Ten Tranquilizers and Their Metabolites in Aquatic Products by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 7, Pages: 833-840(2023)
- 作者机构：
  
  农业农村部渔业环境及水产品质量监督检验测试中心（广州），中国水产科学研究院南海水产研究所，广东广州 510300
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23040604
  CLC：
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王旭峰,王强,张英侠等.超高效液相色谱－串联质谱法同时测定水产品中10种镇静剂及其代谢物残留[J].分析测试学报,2023,42(07):833-840.

WANG Xu-feng,WANG Qiang,ZHANG Ying-xia,et al.Simultaneous Determination of Ten Tranquilizers and Their Metabolites in Aquatic Products by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):833-840.
王旭峰,王强,张英侠等.超高效液相色谱－串联质谱法同时测定水产品中10种镇静剂及其代谢物残留[J].分析测试学报,2023,42(07):833-840. DOI： 10.19969/j.fxcsxb.23040604.

WANG Xu-feng,WANG Qiang,ZHANG Ying-xia,et al.Simultaneous Determination of Ten Tranquilizers and Their Metabolites in Aquatic Products by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):833-840. DOI： 10.19969/j.fxcsxb.23040604.

摘要

建立了测定水产品中10种镇静剂及其代谢物的通过式固相萃取（SPE）/超高效液相色谱－串联质谱（UPLC－MS/MS）多残留分析方法。样品经1%氨水－乙酸乙酯提取，KNORTH m-PFC SPE小柱一步式净化。洗脱液经氮气吹干浓缩，0.5 mL乙腈溶解残渣，采用UPLC－MS/MS测定。目标物采用JADE－PAK KP－C,18,（100 mm × 2.1 mm，1.7 μm）色谱柱分离，以0.1%甲酸－乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱。电喷雾电离正离子（ESI,+,）扫描，多反应监测（MRM）模式下检测，以保留时间和离子丰度比定性，内标法定量。10种目标物在对应质量浓度范围内呈良好的线性关系，相关系数（,r,2,）大于0.999，检出限和定量下限分别为0.1 ~ 0.15 μg/kg和0.3 ~ 0.5 μg/kg。在4种水产品基质中进行3个浓度水平的加标实验，平均加标回收率为82.6% ~ 117%，相对标准偏差（RSD，,n ,= 6）为1.5% ~ 9.3%。该方法灵敏度高、适用性强，适用于不同水产品基质中镇静剂及其代谢物残留的分析。

Abstract

A multi-residue analytical method was established for the simultaneous determination of ten tranquilizers and their metabolites in aquatic products by pass-through solid phase extraction（SPE） in combination with ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．Samples were extracted with 1% ammonium hydroxide－ethyl acetate，followed by one-step cleanup based on KNORTH m-PFC SPE cartridge．The purified extractions were blew to dryness under nitrogen gas．The dried residues were dissolved with 0.5 mL acetonitrile and then injected into UPLC－MS/MS．The chromatographic separation of ten target analytes were conducted on a JADE－PAK KP－C,18, column（100 mm × 2.1 mm，1.7 μm） by gradient elution，utilizing 0.1% formic acid－acetonitrile and 0.1% formic acid solution as mobile phases．The targeted analytes were analyzed with positive electrospray ionization under multiple reaction monitoring（MRM） mode，confirmed using ion ratio and retention time，and quantitated by internal standard method．Excellent linearities for ten target analytes were obtained in the corresponding mass concentration ranges，with correlation coefficients（,r,2,） larger than 0.999．The limits of detection and the limits of quantitation for aquatic product samples were in the range of 0.1－0.15 μg/kg and 0.3－0.5 μg/kg，respectively．The average recoveries for four negative aquatic product matrixes at three spiked levels ranged from 82.6% to 117%，with relative standard deviations（RSDs，,n ,= 6） of 1.5%－9.3%．The proposed method is sensitive and versatile，and it can be applied to the multi-residue analysis of ten tranquilizers and their metabolites in various aquatic product matrixes.

关键词

镇静剂代谢物通过式固相萃取超高效液相色谱－串联质谱水产品

Keywords

tranquilizersmetabolitepass-through solid phase extractionultra-performance liquid chromatography－mass spectrometryaquatic product

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