液相色谱-串联质谱法测定鸡饲料中硝基咪唑类药物
LC-MS/MS Determination of Nitroimidazoles in Poultry Feed
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摘要: 提出了鸡饲料中5种硝基咪唑类药物(甲硝唑、洛硝哒唑、二甲硝唑、替硝唑和奥硝唑)的液相色谱-串联质谱分析方法.鸡饲料样品经乙酸乙酯-5 g·L-1碳酸钠混合溶液提取后,取有机相蒸发至干.用0.1 mol·L-1磷酸溶液溶解残余物,HLB柱固相萃取净化,所得的乙腈洗脱液经C8色谱柱为分离柱,甲醇和水混合溶液为流动相作梯度淋洗,采用正离子模式多反应监测.5种硝基咪唑类药物的线性范围均为10~500 μg·L-1,检出限(3S/N)均为10 μg·kg-1.加标回收率为79.4%~91.3%,批内相对标准偏差(n=6)为5.5%~13.9%,批间相对标准偏差(n=6)为6.7%~18.2%.Abstract: LC-MS/MS was applied to the determination of nitroimidazoles (metronidazole;ronidazole;dimetridazole;tinidazole and ornidazole) in poultry feed.Nitroimidazoles in poultry feed were extracted with a mixed solution of ethyl acetate and 5 g·L-1 Na2CO3 solution,and the organic phase obtained was evaporated to dryness.The residue was desolved with 0.1 mol·L-1 phosphoric acid,and purified by HLB SPE column.The eluate in acetonitrile was used for LC-MS-MS determination,in which C8 column was used as chromatographic column,and a mixture of methanol and water was used as mobile phase in gradient elution;positive electrospray ionization as well as multiple reaction monitoring mode was used in the detection.Linearity ranges of 5 nitroimidazoles were found between 10-500 μg·L-1 with their detection limits (3S/N) of 10 μg·kg-1.Values of recovery found by standard addition method were in the range of 79.4%-91.3%,and values of intra-batch and inter-batch RSD′s (n=6) found were in ranges of 5.5%-13.9% and 6.7%-18.2% respectively.