气相色谱法测定甘氨酰胺盐酸盐中氯乙酸甲酯的含量

摘要

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×0.25μm), 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.%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×0.25μm)，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0.00800~0.12833 mg/ml (r=0.9995)；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。