高效液相色谱-串联质谱法测定动物源食品中氯霉素残留

Determination of chloramphenicol residues in animal derived food by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  动物源食品  氯霉素

英文关键词:high performance liquid chromatography-tandem mass spectrometry  animal derived food  chloramphenicol

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定几种动物源食品中氯霉素残留的方法。方法 对《动物源食品中氯霉素残留量的测定 高效液相色谱-串联质谱法》(农业部第781号公告)中的测定方法进行优化, 样品经提取后经HLB固相萃取小柱净化, 采用甲醇-水进行梯度洗脱, 经Agilent Eclipse-plus C18色谱柱 (3.0 mm×100 mm, 1.8 μm)分离, 采用多反应检测负离子模式进行定性及定量分析。结果 在0.5~10.0 ng/mL范围内, 氯霉素的浓度和色谱峰面积线性关系良好(r=0.9998), 方法检出限为0.03 μg/kg, 定量限为0.1 μg/kg, 在1.0、2.0和5.0 ng/mL 3个水平的加标回收率为91.58%~109.52%, 相对标准偏差小于7.5%。结论 该方法快速、准确、灵敏, 能满足几种动物源食品中氯霉素残留的测定。

英文摘要:

      Objective To establish a method for the determination of chloramphenicol residues in animal derived food by high performance liquid chromatography-tandem mass spectrometry. Methods The method of Determination of chloramphenicol residues in food of animal origin-High performance liquid chromatography-tandem mass spectrometry (Announcement No. 781 of the Ministry of Agriculture) was optimized. The animal derived food sample was extracted, then the extraction liquid was purified by HLB solid phase extraction column. The obtained target compound was separated with Agilent Eclipse-plus C18 (3.0 mm×100 mm, 1.8 μm) column using methanol-water for gradient elution, and then were qualitatively and quantitatively analyzed by using the multi-reaction detection negative ion mode. Results The concentration of chloramphenicol had a good linear relationship with the chromatographic peak area in the range of 0.5?10.0 ng/mL (r=0.9998). The limit of detection was 0.03 μg/kg, and the limit of quantitation was 0.1 μg/kg. The recoveries were ranged from 91.58% to 109.52% for the chloramphenicol residues with three spiked levels of 1.0, 2.0 and 5.0 ng/mL. The relative standard deviations (RSDs) were less than 7.5%. Conclusion This method is fast, accurate and sensitive, which is suitable for the detection of chloramphenicol residual in several animal derived foods.