UPLC-MS-MS法快速测定含乳冷冻饮品中氯霉素残留量

Determination of Chloramphenicol Residue in Contain Milk Frozen Drinks by UPLC-MS-MS

建立了UPLC–MS–MS法测定含乳冷冻饮品中氯霉素的含量。样品经高氯酸沉淀蛋白,乙酸乙酯提取,浓缩干燥,流动相溶解,正己烷脱脂后,采用ACQUITY UPLC BHE C18色谱柱分离,以1%甲酸水溶液–乙腈为流动相进行梯度洗脱,利用电喷雾质谱负离子监测模式对氯霉素进行检测。氯霉素浓度在0.1～100.0 ng/mL范围内与色谱峰面积呈良好的线性,线性相关系数r=0.9986。加标回收率为81.5%～103.4%,测定结果的相对标准偏差为1.72%～3.18%(n=5),以3倍信噪比计算方法的检出限为0.1μg/kg。

The method was established for the determination of chloramphenicol residues in milk-containing frozen drinks by liquid chromatography electrospray ionization mass spectrometry （UPLC-MS-MS）. Protein in samples was precipitated with perchloric acid, extracted with ethyl acetate, then concentrated and dried, dissolved in mobile phase solvent and defated with hexane. The separation was performed on a ACQUITY UPLC BEH Cl8 column with gradient elution using 1% formic acid aqueous solution-acetonitrile. Concentration of chloramphenicol was linear with chromatographic peak area in the range of 0.1-100.0 ng/mL, correlation coefficient r=0. 998 6. The recoveries were 81.5%-103.4%. The relative standard deviation of detection results was 1.72%-3.18% and detection limit was 0.1 μ g/kg （S/N = 3 ）.