顶空气相色谱法测定盐酸乙胺丁醇中的残留溶剂

Determination of Residual Solvents in Ethambutol Hydrochloride by Headspace Gas Chromatography

目的建立GC法同时测定盐酸乙胺丁醇中乙醇、1,2-二氯乙烷2种有机溶剂的残留量。方法采用顶空气相色谱法。色谱柱为J&W DB-SELECT 624UI(30 m×0.32 mm×1.80μm),程序升温,起始温度40℃,维持6 min,以10℃·min^(-1)的速率升温至60℃,维持2 min,再以4℃·min^(-1)的速率升至100℃;进样口温度为200℃,检测器温度为250℃;载气为氮气,流速1 mL·min^(-1);分流比为1∶1;进样方式为顶空进样,顶空平衡温度:65℃,平衡时间为30 min。结果2种待测残留溶剂分离度良好,空白溶剂无干扰。乙醇、1,2-二氯乙烷线性范围分别为101.10~2021.98μg·mL^(-1)(r=0.9996)、0.10~2.08μg·mL^(-1)(r=0.9986),定量限为0.91,0.21μg·mL^(-1),检测限为0.45,0.03μg·mL^(-1),乙醇加样平均回收率为99.4%,RSD为0.7%;1,2-二氯乙烷加样平均回收率为101.1%,RSD为0.6%。结论该方法操作简单、灵敏度高、重复性好,适用于盐酸乙胺丁醇中残留溶剂的测定。

OBJECTIVE To establish a GC method for the simultaneous determination of ethanol and 1,2-dichloroethane residues in ethambutol hydrochloride.METHODS Headspace gas chromatography was used to determinate.The chromatographic column was J&W DB-SELECT 624 UI(30 m×0.32 mm×1.80μm).The temperature was programmed.The initial temperature was 40℃maintaining for 6 min,then increased to 60℃at a rate of 10℃·min^(-1) maintaining for 2 min,and increased to 100℃at a rate of 4℃·min^(-1).The sample port temperature was 200℃,The detector temperature was 250℃.The carrier gas was nitrogen.The flow rate was 1 mL·min^(-1).The split ratio was 1∶1.Headspace injection,equilibrium temperature was 65℃,and the equilibrium time was 30 min.RESULTS The resolution of the two residual solvents to be tested was good,and the blank solvent had no interference.The linear ranges of ethanol and 1,2-dichloroethane were 101.10-2021.98μg·mL^(-1)(r=0.9996),0.10-2.08μg·mL^(-1)(r=0.9986).The limit of quantification were 0.91μg·mL^(-1) and 0.21μg·mL^(-1),respectively.The detection limit were 0.45μg·mL^(-1),0.03μg·mL^(-1),respectively.The average recovery of ethanol was 99.4%,the RSD was 0.7%.The average recovery of 1,2-dichloroethane was 101.1%and the RSD was 0.6%.CONCLUSION This method is simple to operate,highly sensitive,and reproducible.It is suitable for the determination of residual solvents in ethambutol hydrochloride.