GC-MS法测定罗红霉素中的2-甲氧基乙氧基甲基氯  

Determination of 2-methoxyethoxymethyl chloride in Roxithromycin by GC-MS

作　　者：邓鸣 曾庆花 梁秋霞 彭斌 卢日刚 朱健萍 DENG Ming;ZENG Qinghua;LIANG Qiuxia;PENG Bin;LU Rigang;ZHU Jianping(Guangxi Institute for Drug Control,Nanning,Guangxi,530021 P.R.China;Guilin Pharmaceutical Co.Ltd.,Guilin,Guangxi,541004 P.R.China)

机构地区：[1]广西壮族自治区药品检验研究院,广西南宁530021 [2]桂林南药股份有限公司,广西桂林541004

出　　处：《华西药学杂志》2024年第6期710-712,共3页West China Journal of Pharmaceutical Sciences

基　　金：广西科技重大专项(桂科AA22096025)。

摘　　要：目的采用衍生化GC-MS法测定罗红霉素中潜在遗传毒性杂质2-甲氧基乙氧基甲基氯(MEM)的含量。方法采用异丙醇做溶剂并作为衍生化试剂。衍生物采用HP-5MS UI(30 m×0.25 mm,0.25μm)色谱柱分离,选择离子监测模式检测。结果MEM衍生物在2.412~19.30 ng·mL^(-1)与峰面积的线性关系良好;检测限为0.6μg·g^(-1);回收率为70.1%~90.4%,RSD为9.30%(n=9)。3批罗红霉素样品均未检出MEM衍生物。结论所用方法灵敏度高、专属性强,可用于罗红霉素中潜在遗传毒性杂质MEM的检测。OBJECTIVE To determine the 2-methoxyethoxymethyl chloride(MEM)by derivatization GC-MS method,a potentially genotoxic impurity in Roxithromycin.METHODS Isopropyl alcohol was used as both solvent and derivatization reagent.The derivative were separated by HP-5MS UI(30 m×0.25 mm,0.25μm),and determined by selected ion monitoring mode.RESULTS A good linear relationship was obtained between the peak areas and the concentrations of derivative of MEM chloride in the range of 2.412-19.30 ng·mL^(-1).The recoveries were 70.1%-90.4%,and the RSD was 9.30%(n=9).Limit of detection was 0.6μg·g^(-1).MEM derivative was not detected in three batches of Roxithromycin samples.CONCLUSION The method is sensitive and specific,which can be used for the quality control of MEM in Roxithromycin.

关 键 词：罗红霉素 2-甲氧基乙氧基甲基氯 衍生化 异丙醇 含量测定 气相色谱-质谱联用 遗传毒性杂质 

分 类 号：R917[医药卫生—药物分析学]