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目的建立直接提取-超高压液相色谱-电喷雾串联质谱法(UPLC-ESIMS/MS)同时测定原料奶及奶粉中土霉素、四环素、金霉素、强力霉素4种四环素类药物的分析方法。方法原料奶及奶粉样品经少量高氯酸沉淀蛋白、低温冷冻除脂后,用C18色谱柱分离,以0.1%甲酸水和乙腈为流动相进行梯度洗脱,电喷雾串联质谱正离子模式扫描,多反应监测模式(MRM)检测,外标法定量。结果 4种四环素族药物在1～1000ng/mL浓度范围内线性关系良好,相关系数r均在0.993以上。本方法的定量限为(S/N≥10)为原料奶5μg/kg,奶粉25μg/kg,在10、50、100μg/kg三个加标水平下,加标回收率为73.4%～99.4%,相对标准偏差为0.8%～14.3%(n≥6)。结论该方法简便快速、灵敏可靠、经济有效,适用于原料奶及奶粉中土霉素、四环素、金霉素和强力霉素4种四环素族药物残留的测定。
OBJECTIVE To establish simultaneous determination of four kinds of tetracyclines, oxytetracycline, tetracycline, chlortetracycline and doxycycline in raw milk and powdered milk by UPLC-ESIMS / MS method. Methods Raw milk and milk powder samples were precipitated with a small amount of perchloric acid. After cryogenic freezing and degreasing, the samples were separated on a C18 column and eluted with 0.1% formic acid in water and acetonitrile as the mobile phase. Electrospray ionization tandem mass spectrometry (ESI- Multiple reaction monitoring mode (MRM) test, external standard quantitative. Results The linearities of 4 tetracyclines in the concentration range of 1 ~ 1000 ng / mL were good with the correlation coefficients r over 0.993. The limit of quantification (S / N≥10) of the method was 5μg / kg of raw milk and 25μg / kg of milk powder. The recoveries were 73.4% -99.4% under the three spiked levels of 10, 50 and 100μg / , The relative standard deviation was 0.8% ~ 14.3% (n≥6). Conclusion The method is simple and rapid, sensitive, reliable and economical. It is suitable for the determination of four tetracyclines residues of oxytetracycline, tetracycline, chlortetracycline and doxycycline in raw milk and milk powder.