亲水作用色谱-高分辨质谱测定生鲜牛乳中7种氨基糖苷类药物残留

Determination of Seven Aminoglycosides Residues in Raw Cow Milk by HILIC-HRMS

建立了生鲜牛乳中链霉素、双氢链霉素、庆大霉素、妥布霉素、卡那霉素、阿米卡星和安普霉素共7种氨基糖苷类抗生素残留的超高效液相色谱-串联质谱检测方法。样品经100mL/L三氯乙酸-乙腈提取和WCX固相萃取柱净化后,采用亲水作用色谱分离,四极杆-静电场轨道阱高分辨质谱检测。对样品前处理条件、液相色谱流动相及质谱条件进行了优化。结果表明,7种氨基糖苷类抗生素在20μg/L^500μg/L范围内线性关系良好,生鲜牛乳中的加标回收率为88.7%~111.2%,相对标准偏差为6.3%~13.1%,该方法灵敏、准确,可用于生鲜牛乳中多种氨基糖苷类抗生素残留的同时检测。

A ultra-high performance liquid chromatography-transdem mass spectrometry method was developed for the simultaneous determination of seven aminoglycosides residues including streptomycin,dihydrostrepmycin,gentamycin,tobramycin,kanamycin,amkacin and apramycin in raw cow milk.The samples were extracted with 100mL/L trichloroacetic acid aqueous solution and acetonitrile,then the extracts were purified by a WCX cartridge.The seven aminoglycosides residues were seperated by hydrophilic interaction liquid chromatography and detected by high resolution mass spectrometry.The pretreatment condition of the sample,the HPLC condition and the MS operation parameters were optimized.The results showed that the lineareties of the seven aminlglycoside residues in 20μg/L-500μg/L had the correlation coefficient between 0.990 0-0.997 5.The recoveries raged from 88.7%-111.2% with the relative standard deviations of6.3%-13.1%.The proposed method was successfully applied to the determination of the mass concentrations of the analytes in related samples,which provided a sensitive and quantitative method for the quality control of raw milk.This method is effective for the safety monitoring of aminoglycosides residues in raw milk.