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 Residuesin Animal-origin Chinese Medicinal Materials Pheretima and Hirudoin the Retailer by Gas Chromatography

为了建立柱前衍生-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0.1~20μg/L范围内线性关系良好,相关系数r^2≥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、5、10μg/kg这3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、0.1、0.1μg/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。

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 - 20 μg/L, with correlation coefficients not less than 0. 9989. Recoveries of chloramphenicol, thiamphenicol and florfenicol 10 μg/kg were 62.9% - 100.8%, and the relative standard detection（LODs） were 0. 05,0. 1,0. 1 μg/kg respectively. accuracy and precision ,this method could be suitable for the pheretima and hirudo spiked in blank samples at three levels of 1,5, deviation（RSD） was less than 16% ,the limits of With the advantages of simplicity, rapidity, high detection of chloramphenicols medicine residues in pheretima and hirudo.