液相色谱-串联质谱法检测动物组织中阿布拉霉素

目的 建立动物源食品中阿布拉霉素的LC-MS/MS检测方法。方法 待测样品中的阿布拉霉素用5%的三氯乙酸溶液提取, 经MCX固相萃取柱净化、浓缩、定容后采用液相色谱-串联质谱法在正离子模式下检测。结果 该方法在0~5 mg/L范围内有良好的线性关系, 相关系数r>0.995, 在不同基质中, 不同的添加水平下该方法的平均回收率范围在80.9%~101%, 相对标准偏差为1.17%~12.60%; 定量下限为0.030 mg/kg。结论 此方法灵敏度高、准确、重现性好, 适用于动物组织中阿布拉霉素残留量的检测。

Determination of apramycin residues in animal tissues by high pressure liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of apramycin in animal tissues by LC-MS/MS. Methods The residues of apramycin in the test samples were extracted with 5% trichloroacetic acid solution. After being cleaned up with SPE column, concentrated and reconstituted, the residues were detected by liquid chromatography-mass spectrometry under multiple reaction monitoring (MRM) mode via positive-ion mode. Results The method showed a good linearity over the range of 0~5 mg/L for apramycin with r>0.995. The average recoveries were 80.9%~101% at three or four spiked levels in animal tissues, and the relative standard deviations were 1.17%~12.6%. The limit of quantitation was 0.030 mg/kg. Conclusion This method is highly sensitive, accurate and reproducible, and it is suitable for the detection of apramycin in animal tissues.