固相萃取-液相色谱串联质谱法同时测定水产品中3种鱼用麻醉剂残留量

Determination of Three Residues of Anaesthetic for Fish in Aquatic Products by Solid-Phase Extraction with Liquid Chromatography Tandem Mass Spectrometry

建立了固相萃取-液相色谱-电喷雾串联质谱(SPE-HPLC-ESI-MS/MS)测定水产品三卡因、苯佐卡因、喹哪啶3种鱼用麻醉剂残留量的检测方法。样品采用磷酸盐缓冲液-甲醇混合溶液提取,经过Waters Oasis HLB固相萃取柱净化,采用Accucore aQ C18色谱柱分离,以0.1%(v/v)甲酸的水溶液和乙腈溶液作为流动相,梯度洗脱,电喷雾正离子模式下分析检测,外标法定量。3种化合物在1~1000 ng/mL浓度范围内线性良好,相关系数R2均大于0.99,方法的检出限为0.10~0.25 μg/kg。在样品中添加0.5、2、5 μg/kg 3个浓度水平的加标实验中,平均添加回收率在76.8%~93.6%,相对标准偏差(RSD)在2.7%~11.2%,符合残留检测的要求。该方法快速、准确、可靠,适用于水产品中鱼用麻醉剂残留的测定。

A liquid chromatography tandem mass spectrometry (LC–MS/MS) method for determination of residues of tricaine,benzocaine and quinaldine in aquatic products was described.The analytes were extracted with phosphate buffer-methanol mix solution and purified by HLB solid phase extraction column.The separation was performed with Accucore aQ C18 column with the gradient elution of 0.1% formic acid solution and acetonitrile,and finally detected with positive electrospray ionization (ESI+) in multiple reation monitoring (MRM) mode.The external standard calibration curves were used for quantitative analysis.Under the optimal analytical conditions,the linearies of tricaine,benzocaine,quinaldine were in the concentration ranges 1~1000 ng/mL with the correlation coefficients of 0.99 for all the analytes.The limits of detection (S/N=3) of the method were between 0.10 and 0.25 μg/kg.In the spiked experiments with the addition of 0.5,2,5 μg/kg in the sample,the mean spiked recoveries of tricaine,benzocaine,quinaldine recovery rates were 76.8%~93.6%,the relative standards deviation were 2.7%~11.2%.The method was easy,fast,sensitive and accurate,and could satisfied the requirements for determination of three residues of anaesthetic for fish in aquatic products.