【摘要】 建立了液相色谱-电喷雾串联质谱法(LC-ESIMS/MS)测定蜂王浆中10种硝基咪唑类药物残留的分析方法。蜂王浆样品经甲醇沉淀蛋白质,弱碱性条件下乙酸乙酯提取硝基咪唑类药物残留,Oasis(HLB)和C18固相萃取柱净化后,通过液相色谱-质谱联用技术进行检测(正离子方式,多反应监测模式),采用同位素稀释内标法或外标法进行定量。方法的线性范围为5.0~60μg/kg,相关系数大于0.999,在10、20、50μg/kg加标水平的回收率为70%~105%,相对标准偏差小于12.7%,定量下限均为10μg/kg。该方法定量准确,适用于对蜂王浆中硝基咪唑类药物残留的确证检测。更多还原

【Abstract】 Nitroimidazoles and their hydroxy metabolites are banned substances with antibiotic and anticoccidial activity.They are suspected to be carcinogenic and mutagenic.In this paper,a rapid,sensitive and selective method for the determination of ten nitroimidazole residues,including dimetridazole(DMZ),2-hydroxymethyl-1-methyl-5-nitroimidazole(HMMNI) or dimetridazole-OH(DMZOH),metronidazole(MNZ),metronidazole-OH(MNZOH),ronidazole(RNZ),5-nitrobenzimidazole(NBI),ipronidazole(IPZ),ipronidazole-OH(IPZOH),2-methyl-5-nitroimidazole(MNI) and 5-chloro-1-methyl-4-nitroimidazole(CMNI) in royal jelly was established by liquid chromatography-tandem mass spectrometry(LC-ESI MS/MS).Methanol was used to precipitate protein,the supernatant solution was extracted with ethyl acetate under weak basic condition,cleaned up with Oasis(HLB) and C18 columns.The quantitative detection was performed by LC-MS/MS on multiple reaction monitoring(MRM) mode under positive-ion electrospray ionization.The isotope internal standards(D3-DMZOH,D3-DMZ,D3-RNZ,D3-IPZOH,D3-IPZ) were added into the sample solutions,isotope dilution internal standard method or external standard method was used for quantitation analysis.The results showed that the calibration curves of ten nitroimidazole residues were linear in the range of 5.0-60 μg/kg with correlation coefficients more than 0.999.The recoveries of ten nitroimidazole residues at the spiked levels of 10,20 and 50 μg/kg were between 70%and 105%with RSDs less than 12.7%,and the quantitation limits were all 10 μg/kg.The method was specific and accurate,and was suitable for the determination and confirmation of nitroimidazole residues in royal jelly samples.更多还原