LC-MS-MS法同时测定动物肌肉组织和牛奶中10种氨基糖苷类药物的方法优化研究

Simultaneous determination of muscle tissue and milk by LC-MS-MS Study on Optimization of 10 Kinds of Aminoglycoside Drugs

应用高效液相色谱-串联质谱法,建立了动物肌肉组织和牛奶中壮观霉素、潮霉素B、链霉素、双氢链霉素、丁胺卡那霉素、卡那霉素、安谱霉素、妥布霉素、新霉素、庆大霉素10种氨基糖苷类药物的的检测方法。样品通过三氯乙酸提取并沉淀蛋白,用HLB固相萃取柱净化,通过SILICA SG80 S5色谱柱分离,在正离子多反应监测模式下分析定量。在0.02~1μg/mL的浓度范围内线性良好,相关系数大于0.995,在100、200、300μg/kg添加水平下,平均回收率为70%~110%,相对标准偏差均小于15%,检测限为20μg/kg。该方法简单,快速,准确,同时避免七氟丁酸等离子对试剂对仪器造成的污染及离子抑制问题。

A method for the determination of spectinomycin,hygromycin B,streptomycin,dihydrostreptomycin,amikacin and kanamycin in animal muscle tissues and milk was established by high performance liquid chromatography-tandem mass spectrometry,10-aminoglycosides of anthracycline,tobramycin,neomycin and gentamicin.The samples were extracted by trichloroacetic acid and precipitated proteins were purified by HLB solid-phase extraction（SPE） column,separated by SILICA SG80 S5 and analyzed quantitatively in positive ion multiple reaction monitoring mode.The average recoveries were between 70%and 110%with the relative standard deviations（RSDs） of less than 15%,and the detection limits（LOD） were in the range of 0.02~1μg/mL,the correlation coefficient was more than 0.995 and 100,200,300μg/Kg.Mu]g/Kg.The method is simple,rapid and accurate,at the same time,it can avoid the contamination and ion suppression caused by the reagent of heptafluorobutyric acid.