GC-MS法检测盐酸雷尼替丁制剂中的20种邻苯二甲酸酯类塑化剂  

Determination of 20 Kinds of Phthalates Elasticizers in Ranitidine Hydrochloride Preparation by GC-MS

作　　者：海丽萍[1] 王雪芹[2] 

机构地区：[1]河南省直属机关第一门诊部,郑州450003 [2]河南省食品药品检验所,郑州450003

出　　处：《中国药房》2013年第1期78-80,共3页China Pharmacy

摘　　要：目的:建立口服固体制剂中邻苯二甲酸酯类塑化剂的检测方法。方法:采用甲醇提取、过滤后进行气相色谱-质谱法分析,对以盐酸雷尼替丁胶囊(片)为模型对象的285批口服固体制剂进行检测。色谱柱为DB-5MS,载气为氦气,流速为1.0ml/min,分流比为10:1,进样口温度为250℃;柱温为程序升温。电子轰击电离方式;电子轰击能为70eV;定性分析采用扫描模式,扫描质量范围为50～650amu;定量测定采用选择离子监测模式。结果:在本试验条件下,20种邻苯二甲酸酯类分离较好,其中18种组分的检测限均>2μg/g,检测质量浓度线性范围均为2～40μg/ml,相关系数均>0.99,RSD均<10%,加样回收率为79%～99%。结论:本法操作简便、准确、分离效果好,可同时检测口服固体制剂中的20种邻苯二甲酸酯类塑化剂。OBJECTIVE：To establish a method for the determination of phthalates elasticizers in oral solid preparation.METHODS：Phthalates were extracted with methanol.285 batches of oral solid preparations,taking Ranitidine hydrochloride capsules or tablets as model subjects,were determined by GG-MS.The determination was performed on DB-5MS column at the flow rate of 1.0 ml/min using helium as carrier gas.The split ratio was 10：1 and injector temperature was 250 ℃ by temperature programming.Electron impact（EI）ionization mode was used with electron bombardment energy of 70 eV;scan mode was adopted for qualitative analysis with scanning range of 50-650 amu;SIR was used for quantity analysis.RESULTS：20 kinds of phthalates could be completely separated under the condition of GC-MS.The linear ranges were 2-40 μg/ml,and relative coefficient was more than 0.99（RSD10%）.The limit of detection was more than 2 μg/g and average recoveries were 79%-99%.CONCLUSION：The method is simple,accurate,well-separated,and could be applied for simultaneous determination of 20 kinds of phthalates elasticizers in oral solid preparation.

关 键 词：气相色谱-质谱法 邻苯二甲酸酯类 塑化剂 盐酸雷尼替丁 胶囊 片剂 

分 类 号：R927.2[医药卫生—药学]