基质固相分散-亲水交互作用色谱-串联质谱法测定牛奶中5种氨基糖苷类抗生素残留量

Determination of 5 aminoglycoside residues in milk by matrix solid phase dispersion-hydrophilic interaction chromatography-tandem mass spectrometry

目的研究亲水交互作用色谱-串联质谱测定牛奶中5种氨基糖苷类抗生素的方法。方法样品经含二氧化硅和乙二胺四乙酸二钠混合材料进行基质固相分散提取后,用含0.1%甲酸的超纯水洗脱,亲水交互作用色谱-串联质谱分析,对样品前处理的模式和条件、色谱分析的固定相和流动相进行优化。结果三个浓度的样品加标试验结果显示,回收率为65.7%~96.5%,相对标准偏差为4.3%~8.6%(n=6),定量限和检出限分别为8.0~80和2.5~25μg/kg。结论建立的分析方法简便、准确、灵敏,满足牛奶中5种氨基糖苷类抗生素残留检测要求。

Objective To establish a method for determination of 5 aminoglycoside residues in milk by hydrophilic interaction chromatography-tandem mass spectrometry. Methods The sample was extracted by matrix solid phase dispersion with silicon and ethylenediaminetetraacetic acid disodium salt. After the elution using 0. 1% formic acid, the sample was detected by hydrophilic interaction chromatography-tandem mass spectrometry. The conditions of elution for mobile phase and analysis for mass spectrometry were optimized. Results The recoveries of three spiked were at 65. 7%- 96. 5% and the relative standard deviations of detection were at 4. 3%-8. 6%( n = 6). The limits of quantification and detection were 8. 0-80 μg/kg and 2. 5-25μg/kg. Conclusion The method is simple, accurate, sensitive and it can meet the determination requirements of drug residues in foods.