口服固体制剂中20种邻苯二甲酸酯类化合物的GC-MS法测定

目的: 建立口服固体制剂中邻苯二甲酸酯类化合物的测定方法。 方法: 采用甲醇提取,过滤,DB-5MS色谱柱(30 m×0.25 mm×0.25 μm),氦气为载气,流速1.0 mL·min^-1,GC-MS联用法检测,检测方式为SCAN和SIR。 结果: 实验条件下,20种邻苯二甲酸酯类能很好分离检测,各组分的检出限均大于2 μg·g^-1,线性范围均在2~40 μg·mL^-1之间,相关系数均大于0.99,RSD均小于10%,加标回收率在79%~99%之间。 结论: 本法对色谱柱和仪器污染小,进样残留少,可同时测定口服固体制剂中的20种邻苯二甲酸酯类化合物。

Objective: To establish a GC-MS method for simultaneous determination of 20 types of phthalates in oral preparation. Methods: Phthalates were extracted with methanol.The analysis was performed by GC-MS SCAN and SIR using DB-5MS column(30 m×0.25 mm×0.25 μm). Results: Totally,20 types of phthalates could be completely separated by GC-MS under the experimental condition.The linear range was 2 μg~40 μg,relative coefficient was more than 0.99,RSD was less than 10%,and average recovery was 79%~99%. Conclusion: This detection method could be applied in the determination of phthalates esters in oral preparation.