GC法测定氯化乙酰甲胆碱中的乙醛和环氧丙烷  

Determination of acetaldehyde and propylene oxide in Methacholine chloride by GC method

作　　者：彭丽娇 李文明 赵春杰[1] 赵旻[1] PENG Lijiao;LI Wenming;ZHAO Chunjie;ZHAO Min(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang,Liaoning,110016 P.R.China;Beijing Tide Pharma-ceutical Co.,Ltd.,Beijing,100023 P.R.China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]北京泰德制药股份有限公司,北京100023

出　　处：《华西药学杂志》2025年第2期178-180,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用GC法检测氯化乙酰甲胆碱中基因毒性杂质乙醛和环氧丙烷的限量。方法采用DB-WAX色谱柱(30 m×320μm,0.5μm),检测器温度250℃,进样口温度150℃,柱流速1.5 mL·min^(-1);采用程序升温,起始温度为40℃,维持3 min,以15℃·min^(-1)升至50℃,再以30℃·min^(-1)升至240℃,维持3 min;以顶空瓶平衡温度85℃,平衡15 min作为顶空条件。结果乙醛和环氧丙烷分离良好;乙醛的检测限为0.08μg·mL^(-1),加样回收率为90.27%~102.40%,在0.27~3.0μg·mL^(-1)与峰面积的线性关系良好(r=0.9992);环氧丙烷的检测限为0.10μg·mL^(-1),加样回收率为79.25%~87.91%,在0.33~3.00μg·mL^(-1)与峰面积的线性关系良好(r=0.9992)。结论所用方法操作简单,准确度高,可用于氯化乙酰甲胆碱原料中乙醛和环氧丙烷的检测。OBJECTIVE To determine the genotoxic impurity acetaldehyde and propylene oxide in Methacholine chloride.METHODS The determination was performed on DB-WAX(30 m×320μm,0.5μm)column.The temperature of the injection port was maintained at 150℃and that of detector at 250℃.Column flow rate was set at 1.5 mL·min^(-1).The column temperature and the initial temperature was set at 40℃and maintained for 3 min,and then the temperature was raised to 50℃at a rate of 15℃·min^(-1).The temperature was raised to 240℃at a rate of 30℃·min^(-1),which maintained for 3 min.The injection volume was 1 mL.RESULTS Acetaldehyde and propylene oxide were finely separated.The LOD of acetaldehyde was 0.08μg·mL^(-1),the recovery rate was 90.27%-102.40%,showing good linearity in range of 0.27-3.00μg·mL^(-1),and the linear correlation coefficient was 0.9992.The LOD of propylene oxide was 0.10μg·mL^(-1).The recovery rate was 79.25%-87.91%.Good linearity existed in range of 0.33-3.00μg·mL^(-1),and the linear correlation coefficient was 0.9992.CONCLUSION The method is rapid and accurate,which is suitable for the determination of acetaldehyde and propylene oxidin.

关 键 词：氯化乙酰甲胆碱 乙醛 环氧丙烷 气相色谱 顶空 基因毒性 限量检查 

分 类 号：R917[医药卫生—药物分析学]