高效液相色谱-串联质谱联用测定蜂王浆中硝基咪唑类药物残留

Optimization of Nitromidazoles Residues in Royal Jelly by Liquid Chromatography Tandem Mass Spectrometry

本文研究了用2%高氯酸提取、乙酸乙酯反萃取,正己烷脱脂进行样品净化,液相色谱-串联质谱同时测定蜂王浆中甲硝唑、洛硝哒唑、二甲硝咪唑三种硝基咪唑类药物残留的检测方法。采用Agilent 1200高效液相色谱仪、API 3200串联四极杆质谱仪对甲硝唑、洛硝哒唑、二甲硝咪唑等3种药物进行了测定条件优化,三种药物在0.1～20μg·kg-1范围内线性关系良好(r>0.9990);以0.5、5、20μg·kg-1浓度水平的添加回收率为90.5%～127%,日内变异系数≤11.4%,日间变异系数≤14.6%。本方法检测定量限(S/N=10):甲硝唑0.1μg/kg,洛硝哒唑0.2μg/kg,二甲硝咪唑0.1μg/kg,可作为硝基咪唑类药物在蜂王浆中残留的快速检测方法。

A optimization method was developed for determination of 3 nitromidazoles,metronidazole,ronidazole and dimetridazole in royal jelly using Agilent 1200 liquid chromatography and API 3200 tandem mass spectrometry. Royal jelly was extracted by 2%perchloric acid and then counter extraction with acetic ether and then degreasing with hexane.The determination of purified samples were achieved by liquid chromatography tandem mass spectrometry.The procedure was validated by spiking 3 nitromidazoles(metronidazole,ronidazole and dimetridazole ) at 3 levels(0.5,5, 20μg·kg-1 ):linearity(r>0.9990 ),accuracy(recovery=90.5%-127%),precision(intra-day CV≤11.4%,interday CV≤14.6%) and sensitivity(metronidazole and dimetridazole LOQ=0.1μg/kg,ronidazole LOQ=0.2μg/kg ) were met the requirement of method for determination of nitromidazoles residues.The results showed that this method was a highly productive procedure for optimization of the nitromidazoles residues in royal jelly.