顶空气相色谱法检测苄星青霉素原料药中的5种残留溶剂

目的：建立检测苄星青霉素原料药中5种残留溶剂（甲醇、乙醇、乙酸乙酯、正丁醇、乙酸丁酯）的方法。方法：以二甲基亚砜为溶剂,采用顶空气相色谱法,色谱柱为DB-624;程序升温;载气为氮气,流速为4.5mL·min-1;进样口温度为200℃;氢离子火焰检测器温度为250℃;顶空瓶平衡温度为80℃,平衡时间为30min。结果：5种残留溶剂峰分别与相邻峰分离完全,在各自的浓度范围内与峰面积呈良好的线性关系（r为0.9990～0.9993）,加样回收率为97.9%～103.1%,RSD为1.1%～2.4%（n=9）,最低检测限为0.5～1.2μg·mL-1。结论：该方法简便、准确、灵敏,可用于苄星青霉素原料药中残留溶剂的检测。

Determination of Five Residual Solvents in Benzylpenicillin Benzathine Crude Material Drug by Head-space Gas Chromatography

OBJECTIVE：To establish a method for determination of five residual solvents（methanol,ethanol,ethylacetate,n-butanol,butylacetate） in benzylpenicillin benzathine crude material drug.METHODS：Head-space gas chromatography method was used with a DB-624 column,with temperature programming,using nitrogen as carrier gas at the flow rate of 4.5 mL·min-1.The injector temperature was 200 ℃,and the FID detector temperature was 250 ℃.Head-space oven was set a temperature of 80 ℃ for 30 min.DMSO was the solvent.RESULTS：The peaks of five residual solvents could be completely separated from the other peaks respectively.Linear responses were obtained for the five residual solvents in their respective concentration ranges（r were 0.999 0～0.999 3）.The recoveries were between 97.9% and 103.1%,RSD were 1.1%～2.4%（n=9）,The LOD were between 0.5 and 1.2μg·mL-1.CONCLUSIONS：The method is simple,accurate and sensitive.It could be used for determination of residual solvents in benzylpenicillin benzathine crude material drug.