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

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

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-C18(100 mm×2.1 mm,1.7μm)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(r2)大于0.999,检出限和定量下限分别为0.1~0.15μg/kg和0.3~0.5μg/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。

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 clean⁃up based on KNORTH m-PFC SPE cartridge.The purified extractions were blew to dryness under nitro⁃gen 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-C18 column(100 mm×2.1 mm,1.7μm)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 electro⁃spray 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 ob⁃tained in the corresponding mass concentration ranges,with correlation coefficients(r2)larger than 0.999.The limits of detection and the limits of quantitation for aquatic product samples were in the range of 0.1-0.15μg/kg and 0.3-0.5μg/kg,respectively.The average recoveries for four negative aquat⁃ic 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.