【摘要】 将微波辅助衍生法与离子液体分散液液微萃取法相结合,建立了牛奶中链霉素、庆大霉素、卡那霉素、妥布霉、小诺霉素、阿米卡星和新霉素等7种氨基糖苷类抗生素(AGs)的快速萃取、衍生方法。本研究以氯甲酸芴甲酯(FMOC-Cl)为衍生试剂,1-辛基-3-甲基咪唑六氟磷酸盐(Omim]PF6)为提取剂,甲醇为分散剂,将微波辅助衍生和离子液体分散液液微萃取相结合,使目标化合物被衍生的同时被萃取和富集到离子液体中,并通过高效液相色谱荧光检测器进行定量检测。实验结果表明,各化合物在线性范围内具有较好的线性关系(r>0.9989),检出限为0.11~0.57μg/L。加标样品回收率在91.95~106.33%之间,其RSD为1.39~5.92%。本法操作简单,灵敏度高,结果可靠,可广泛应用于牛奶样品中氨基糖苷类抗生素的检测。更多还原

【Abstract】 A new method based on simultaneous microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction was developed for the derivatization and extraction of aminoglycosides(AGs) including streptomycin(STR), gentamicin(GEN), kanamycin(KAN), tobramycin(TOB), micronomicin(MIC), amikacin(AMI) and neomycin(NEO) in milk samples. In the experiment, 9-fluorenylmethyl chloroformate(FMOC-Cl), 1-octyl-3-methylimidazolium hexafluorophosphate([Omim]PF6) and methanol were used as derivatization reagent, extraction solvent and disperser, respectively. Aminoglycosides were simultaneously derivatized and extracted into ionic liquid phase by this method in a single step. Derivatives of the aminoglycosides were then determined by high-performance liquid chromatography coupled with fluorescence detection. The calibration curve had good linear relationship(r>0.9989). The limits of detection(LODs) of analytes were in range of 0.11~0.57 μg/L. The recoveries were between 91.95% and 106.33% with the relative standard deviations of 1.39~5.92%. The proposed method has the advantages of simple operation, high sensitivity and reliable results and should be extensively applied for determination of aminoglycosides in milk samples.更多还原