GC法测定市售动物源性中药材地龙、水蛭中3种氯霉素类药物的残留量

Determination of 3 Chloramphenicols Medicine Residues in animal-origin Chinese medicinal materials Pheretima and Hirudo in the retailer by Gas Chromatography

关键词:  中药材  地龙  水蛭  氯霉素类药物  残留量  气相色谱

Key words:  Chinese medicinal materials  Pheretima  Hirudo  Chloramphenicols Medicine  Residues  Gas chromatography

摘要:

建立了柱前衍生-GC-ECD法同时测定市售动物源性中药材地龙、水蛭中氯霉素、甲砜霉素、氟甲砜霉素3种氯霉素类抗生素残留量的方法。样品经乙酸乙酯超声提取，旋转蒸干后，提取物溶于4%氯化钠溶液，经正己烷去脂，液液分配净化。再加BSTFA-TMCS衍生化反应后氮气吹干，正己烷定容进样分析，外标法定量。结果表明，氯霉素、甲砜霉素和氟甲砜霉素在0.1 μg/L～20 μg/L范围内线性关系良好，相关系数r2≥0.9989；空白样品加标实验表明，氯霉素、甲砜霉素和氟甲砜霉素在1 μg/kg、5 μg/kg、10 μg/kg3个添加水平下的回收率为62.9%～100.8%，RSD＜16%，其检出限分别为 0.05 μg/kg、0.1 μg/kg、0.1 μg/kg。该方法简便快捷，准确度和精密度高，适用于地龙、水蛭中氯霉素类药物的残留测定。

Abstract:

Pre-column derivatization GC-ECD method was established to simultaneously determine the residues of chloramphenicol(CAP)，thiamphenicol(TAP) and florfenicolin(FF) in animal-original Chinese medicinal materials Pheretima and Hirudo in the retailer．The samples were extracted with ethylacetate by ultrasound assistance and evaporated to dry．The extracts were dissolved in 4% sodium chloride solution，defatted with n-hexane，and cleaned up by liquid-liquid partition．The purified extracts were derivatized with BSTFA-TMCS and derivatization solution was dried under nitrogen．The final targets were dissolved with n-hexane and quantitatived by external standard method．The results indicated that the calibration curves of chloramphenicol, thiamphenicol and florfenicol were linear in the ranges of 0.1 μg/L～20 μg/L，with correlation coefficients not less than 0.9989；Recoveries of chloramphenicol, thiamphenicol and florfenicol spiked in blank samples at three levels of 1 μg/kg、5 μg/kg、10 μg/kg were 62.9%～100.8%，and the relative standard deviation(RSD) was less than 16%，the limits of detection(LODs) were 0.05 μg/kg，0.1 μg/kg，0.1 μg/kg respectively．With the advantages of simplicity，rapidity，high accuracy and precision，this method could be suitable for the detection of chloramphenicols medicine residues in Pheretima and Hirudo．