通过式固相萃取净化/液相色谱-串联质谱法快速检测水产品中11种青霉素残留

采用通过式固相萃取净化策略去除样品基质中的脂肪和磷脂等杂质干扰,结合液相色谱-串联质谱检测,建立了水产品中11种青霉素残留的同时快速分析方法。样品经80%乙腈水溶液提取,Oasis PRi ME HLB通过式固相萃取柱净化,C_(18)色谱柱分离,0.05%甲酸乙腈溶液和0.05%甲酸水溶液梯度洗脱,多反应监测正离子模式扫描,内标法定量。11种目标物在相应浓度范围内线性关系良好,相关系数不低于0.99,检出限为0.30~1.5μg/kg。基质加标回收率为85.5%~110%,相对标准偏差(RSD)为5.9%~14.3%。该方法前处理操作简便,灵敏度和准确度高,可实现水产品中多种青霉素药物残留的同时快速测定。

Rapid and Simultaneous Determination of 11 Penicillin Residues in Fishery Products by Pass through SPE Purification and Liquid Chromatography-Tandem Mass Spectrometry

A method was developed for the rapid and simultaneous determination of 11 penicillins in fishery products by pass-through SPE purification with liquid chromatography tandem mass spectrometry(LC-MS/MS).The samples were extracted with acetonitrile-water (80 ∶ 20,by volume),and then cleaned up with an Oasis PRiME HLB pass-through SPE column.The separation of 11 penicillins were performed on a Kinetex XB-C1s(2.1 mm × 100 mm,2.6 μm) column by using a mixture of 0.05％ formic acid and acetonitrile containing 0.05％ formic acid as mobile phase.Qualitative and quantitative analyses of the analyte were carried out under the multiple reaction monitoring (MRM) mode with positive electrospray ionization.And the isotope internal standards were employed for the quantification.The calibration curves were linear well in corresponding concentration ranges,with correlation coefficient over 0.99.The detection limits ranged from 0.30 μg/kg to 1.5 μg/kg.The average spiked recoveries for 11 penicillins werc between 85.5％ and 110％ with relative standard deviations(RSDs) of 5.9％-14.3％.The proposed method is accurate,sensitive and high-efficient,and is practical for the determination of penicillins in fishery products.