顶空液相微萃取-气相色谱法测定阿奇霉素中二氯甲烷和丙酮残留量

Determination of Dichloromethane and Acetone Residues in Azithromycin by Headspace Liquid Phase Microextraction Coupled with Gas Chromatography

采用液相微萃取与气相色谱联用技术测定阿奇霉素中二氯甲烷和丙酮的残留量。以苯乙酮为萃取溶剂,萃取时间30 min,萃取温度60℃,萃取液滴体积2μL。在浓度为20.0μg/g^120.0μg/g范围内,二氯甲烷的外标曲线为Y=0.009 9X-0.088 2,相关系数R^2=0.983 1;丙酮的外标曲线为Y=0.029 1X-0.040 5,相关系数R^2=0.9865;阿奇霉素中丙酮测定结果的相对标准偏差(RSD%)为1.19,加标回收率为93.49%~101.1%;方法的最低检测限:二氯甲烷为0.298μg/g,丙酮为0.059μg/g。

A method was used for the determination of residual dichloromethane and trichloromethane in ranitidine hydrochloride by liquid phase microextraction coupled with gas chromatography（ GC）. Acetophenone was as extraction solvent,the extraction time was 30 min,the extraction temperature was 60 ℃,the extraction liquid drop volume was 2 μL. The external standard curve of dichloromethane was Y = 0. 009 9X- 0. 088 2,the correlation coefficient was R^2= 0. 983 1 and the external standard curve of acetone was Y = 0. 029 1X- 0. 040 5,the correlation coefficient was R^2= 0. 9865 within the concentration ranges of dichloromethane（ 20. 0 μg / g ~ 120. 0 μg / g）. The relative standard deviation（ RSD%） of the determination of acetone in azithromycin was 1. 19. The recovery rate was in the range of 93. 49% ~ 101. 1%. The lowest detection limit of method were as follows： the dichloromethane was 0. 298μg / g,the acetone was 0. 059 μg / g.