高效液相色谱-串联质谱法快速测定动物源食品中的氯霉素残留量

Rapid determination of chloramphenicol residue in animal derived food by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  氯霉素  动物源食品  内标法

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

中文摘要:

      目的 建立高效液相色谱-串联质谱联用法快速测定动物源食品中氯霉素残留量的分析方法。方法 样品采用乙酸乙酯提取、空气吹干浓缩、正己烷脱脂后, 经乙腈和水梯度洗脱、色谱柱Poroshell 120 EC-C18 (50 mm×2.1 mm, 2.7 μm)分离、液相色谱-串联质谱仪测定, 以氘代氯霉素为内标物进行定量。结果 回归方程Y=0.177X+0.0008, 相关系数r为0.9996; 方法检出限和定量限分别为0.03 μg/kg、0.1 μg/kg; 在0.1~1.0 μg/kg浓度梯度范围内的平均回收率为91.4%~107.5%, 相对标准偏差为4.5%~5.7%, 2次能力验证结果满意。结论 该方法经济、简便、快捷、稳定、准确性高, 能满足大批量动物源性食品样品中氯霉素残留量测定的要求。

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 (HPLC-MS/MS). Methods The animal derived food sample was extracted by ethyl acetate, the extraction liquid was enriched by air flow, and purified by n-hexane. The obtained target compound was separated by high performance liquid chromatography using Poroshell 120 EC-C18 (50 mm×2.1 mm, 2.7 μm) HPLC column with gradient elution of acetonitrile and water, and was detected by HPLC-MS/MS with multiple reaction monitoring mode (MRM). Internal standard method was used for quantitative analysis, and deuterated chloramphenicol was used for internal standard. Results The regression equation was Y=0.177X+0.0008, and the correlation coefficient r was 0.9996. The limit of detection was 0.03 μg/kg, and the limit of quantitation was 0.1 μg/kg. The recoveries for spiked standards in the concentration range of 0.1-1.0 μg/kg and the relative standard deviations were 91.4%-107.5% and 4.5%-5.7%, respectively. The results of two batches proficiency testing were satisfactory. Conclusion This method is economical, simple, rapid, effective and accurate, which is suitable for the determination of the content of chloramphenicol residue in animal derived food samples.