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目的建立1种超高效液相色谱-串联质谱联用法测定乳制品中8种青霉素类抗生素残留的确证方法。方法乳制品样品用水提取后,经乙腈沉淀蛋白,正己烷液液萃取除去脂肪,用氮气吹至近干,用乙腈+水(10+90)复溶后,经0.22μm微孔滤膜过滤,经Endeavorsil C18柱分离,选用乙腈(含0.1%甲酸)-水(含0.1%甲酸)为流动相,13 min内梯度洗脱分离8种青霉素;在优化的质谱条件下,采用ESI源、正离子模式、多反应监测方式、外标法定量。结果在浓度范围1.0~100.0μg/kg,8种青霉素类药物在各种乳制品基质中均有良好的线性关系,相关系数为0.999 2~0.999 8,方法最低检测限为0.03~0.15μg/kg,方法回收率为91.0%~102.3%,相对标准偏差为1.02%~6.13%。用本研究建立的方法检测78份奶粉、液体牛奶、鲜奶、奶饮料样品,其中3份样品检出青霉素G,含量为0.2~1.6μg/kg。结论该方法测定牛奶中8种青霉素药物的残留量简便、快速、准确,可以满足对牛奶中青霉素残留的检测要求。
Objective To establish a method for the determination of 8 penicillin antibiotics residues in dairy products by ultra performance liquid chromatography-tandem mass spectrometry. Methods After the dairy products were extracted with water, the proteins were precipitated by acetonitrile and extracted with n-hexane by liquid-liquid extraction. The samples were blown to near dryness with nitrogen, reconstituted with acetonitrile + water (10 + 90), filtered through 0.22 μm microporous membrane, Endeavorsil C18 column was used. Eight kinds of penicillins were separated by gradient elution with acetonitrile (containing 0.1% formic acid) -water (containing 0.1% formic acid) and gradient elution within 13 min. Under optimized mass spectrometry, ESI source and positive ion mode , Multiple reaction monitoring methods, external standard quantitative. Results There was a good linear relationship between the eight penicillins and various dairy matrices in the concentration range of 1.0-100.0 μg / kg with the correlation coefficient of 0.999 2-0.9999 8. The detection limit of the method was 0.03-0.15 μg / kg The recoveries were 91.0% ~ 102.3% with relative standard deviations of 1.02% ~ 6.13%. 78 samples of milk powder, liquid milk, fresh milk and milk beverage samples were detected by the method established in this study. Among them, 3 samples were detected with penicillin G at 0.2-1.6 μg / kg. Conclusion The method is simple, rapid and accurate for the determination of 8 kinds of penicillin residues in milk, which can meet the detection requirements of penicillin residues in milk.