高效液相色谱-质谱联用法测定乳及乳制品中氯霉素类药物残留量

Determination of chloramphenicols residues in milk and dairy products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  氯霉素  甲砜霉素  氟甲砜霉素  乳及乳制品  高效液相色谱-质谱法

英文关键词:chloramphenicol  thiamphenicol  florfenicol  milk and dairy products  liquid chromatography-tandem mass spectrometric

中文摘要:

      目的 建立同时测定乳制品中氯霉素、甲砜霉素和氟甲砜霉素的液质联用方法。方法 样品经乙腈提取, 饱和乙腈正己烷脱脂, 以甲醇水作为流动相, 通过高效液相色谱, 采用负离子模式多反应监测, 氯霉素用同位素内标定量, 甲砜霉素、氟甲砜霉素用外标法定量。结果 本方法线性范围: 0.25~20.0 μg/L, 相关系数＞0.999, 检出限0.01 μg/kg, 定量限0.1 μg/kg, 三种物质添加水平分别为0.5、2.5、5.0 μg/kg, 加标回收率分别为氯霉素82.2~103%, 甲砜霉素81.8~108%, 氟甲砜霉素67.6~104%, RSD<10%。结论 该方法具有简单快速、灵敏度高、准确性强等特点, 适用于测定乳及乳制品中氯霉素、甲砜霉素和氟甲砜霉素的含量。

英文摘要:

      Objective A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis method was established for simultaneous determination of chloramphenicol, thiamphenicol and florfenicol in milk and dairy products. Methods The sample was extracted with acetonitrile and degreased with saturated acetonitrile n-hexane. Mobile phase was methanol and water. The identification and quantification of chloramphenicols residues were carried out by MS/MS in negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode. Using isotope internal standard quantitation of chloramphenicol, thiamphenicol and florfenicol by external standard method for quantitative. Results The calibration curve showed a good linearity in the range of 0.25~20.0 μg/L with the correlation coefficient r2>0.999. The detection limit was 0.01 μg/kg. The quantification (LOQ) limit was 0.1 μg/kg. The average re-coveries of chloramphenicol, thiamphenicol and florfenicol spiked at 0.5, 2.5 μg/kg and 5.0 μg/kg levels in different matrix were 82.2%~103%, 81.8%~108% and 67.6%~104%. The relative standard deviations were less than 10%. Conclusion This method is simple, effective and sensitive, and it is suitable for the determination of chloramphenicol, thiamphenicol and florfenicol in milk and dairy products.