鱼肉中盐酸小檗碱和盐酸氯苯胍残留的快速测定

Fast Determination of Berberine Hydrochloride and Robenidine Hydrochloride in Fish Meat

传统的固相萃取和过膜技术存在操作繁琐、耗时长等问题。本文通过优化相关技术参数,整合通过式固相萃取(PRiME)和微孔滤膜技术,实现进样前操作步骤一体化。利用液相色谱串联质谱建立鱼肉中盐酸小檗碱和盐酸氯苯胍的定量检测方法。方法验证试验结果显示:盐酸小檗碱和盐酸氯苯胍在质量浓度0.5~100μg/L范围内线性关系良好,检出限(LOD)分别是0.51μg/kg和0.53μg/kg,定量限(LOQ)分别是1.67μg/kg和1.68μg/kg,日内精密度相对标准偏差范围分别为4.09%~4.48%和3.84%~3.90%,日间精密度相对标准偏差范围为5.17%~5.73%和4.23%~5.29%。在5,10,50μg/kg 3个水平下,盐酸小檗碱和盐酸氯苯胍的回收率范围分别为91.2%~93.2%和91.3%~92.4%;RSD范围分别为4.5%~4.6%和1.8%~5.2%。采用液相色谱串联质谱法测定市售活鱼中目标化合物残留,未检出阳性样品,说明盐酸小檗碱和盐酸氯苯胍在水产养殖方面使用情况良好,该检测方法符合痕量分析的要求。

Traditional solid-phase extraction(SPE) and membrane filtration technology are complicated,and time and labor consuming.In this study,the PRiME and membrane filtration technology were integrated to realize the integration of operational steps before sample injection,and the relevant technical parameters were optimized.A quantitative method for the determination of berberine hydrochloride and robenidine hydrochloride in fish was established by liquid chromatography tandem mass spectrometry.The results showed that berberine hydrochloride and robenidine hydrochloride had good linearity in the range of 0.5-100 g/L,the detection limits(LOD) were 0.51 g/kg and 0.53 g/kg,the quantitative limits(LOQ) were 1.67 g/kg and 1.68 g/kg,the intraday relative standard deviation of precision was 4.09%-4.48% and 3.84%-3.90%,respectively,and the intraday relative standard deviation of precision was 5.17%-5.73% and 4.23%-5.29%,respectively.The recoveries of berberine hydrochloride and robenidine hydrochloride were 91.2%-93.2% and 91.3%-92.4%,respectively,at 5,10,50 g/kg concentrations.The RSD was 4.5%-4.6% and 1.8%-5.2%,respectively.The liquid chromatography-tandem mass spectrometry(LC-MS) was used to determine the residues of target compounds in fresh fish on the market,and no positive samples were detected,indicating that berberine hydrochloride and chlorophenguanidine hydrochloride were used well in aquaculture.