气相色谱法测定甘氨酰胺盐酸盐中氯乙酸甲酯的含量-海南医学.PDF

海南医学2015年11月第26卷第22期 Hainan Med J, Nov. 2015, Vol. 26, No. 22 doi:10.3969/j.issn.1003-6350.2015.22.1230 ·药物与临床· 气相色谱法测定甘氨酰胺盐酸盐中氯乙酸甲酯的含量 李才岛，韦 华 (海南正瑞医药科技开发有限公司，海南 海口 570311) 【摘要】 目的 建立测定甘氨酰胺盐酸盐中氯乙酸甲酯含量的气相色谱法。方法 采用气相色谱法。色 谱柱为DB-WAX 毛细管柱( 固定液：聚乙二醇；规格：30.0 m×0.25 mm×0.25 μm) ，柱温为110℃，FID 检测器温度为 250 ℃，进样口温度为200 ℃，分流比为10:1，顶空瓶平衡温度为85℃，顶空瓶平衡时间为30 min。结果 氯乙酸 甲酯检测浓度的线性范围为0.008 00~0.128 33 mg/ml (r=0.999 5) ；平均回收率为100.0% (RSD=1.79%)。结论 本方法操作简便快捷，结果准确可靠，可用于甘氨酰胺盐酸盐中氯乙酸甲酯的质量控制。 【关键词】 甘氨酰胺盐酸盐；氯乙酸甲酯；气相色谱法 【中图分类号】 R971 【文献标识码】C 【文章编号】 1003—6350（2015 ）22—3394—03 Contentdeterminationofmethylchloroacetateinglycinamidehydrochloridebygaschromatography. LI Cai-dao,WEIHua.HainanZhengruiMedicalTechnologyDevelopmentCo.,Ltd.,Haikou570311,Hainan,CHINA 【Abstract】 Objective To establish a gas chromatographic method for determining the content of methyl chloroacetate in glycinamide hydrochloride. Methods Gas chromatography (GC) was adopted with DB-WAX capil- lary column (Stationary liquid: polyethylene glycol; Specification: 30.0 m ×0.25 mm ×0.25 μm), column chromatogra- phy of 110 ℃, FID detector temperature of 250℃, injection port temperature of 200℃, split ratio of 10:1, equilibrium temperature of empty bottles of 85 ℃, and equilibrium time of empty bottles of 30 minutes. Results The linear range of methyl chloroacetate detected was 0.008 00~0.128 33 mg/ml (r=0.9995). The average recovery rate was 100.0% (RSD=1.79%). Conclusion This method is fast, easy to operate, accurate and reliable, which can be used in the quali- ty control of methyl chloroacetate in glycinamide hydrochloride. 【Keywords】 Glycinamide hydrochloride; Methyl c