顶空气相色谱法测定替考拉宁原料药及注射剂中5种有机溶剂残留量  

Determination of Residues of 5 Organic Solvents in Teicoplanin Raw Material and Injection by Headspace GC

作　　者：耿文飞[1] 吴军营[1] 王春霞 任乐民 可爱兵[1] 

机构地区：[1]华北制药集团新药研究开发有限责任公司/微生物药物国家工程研究中心/河北省工业微生物代谢工程技术研究中心,石家庄050015 [2]河北省食品药品检验院,石家庄050011

出　　处：《中国药房》2015年第18期2554-2556,共3页China Pharmacy

摘　　要：目的：建立测定替考拉宁原料药及注射剂中5种有机溶剂残留量的方法。方法：采用顶空气相色谱法。色谱柱为以6%氰丙基苯基-94%二甲基聚硅氧烷（DB-624）为固定液的毛细管柱,采用程序升温,进样口温度为200℃,检测器为氢火焰离子化检测器（FID）,载气为高纯氮气,恒定流速为1 ml/min,分流比为40∶1,进样量为1 ml。结果：乙醇、丙酮、乙酸乙酯、四氢呋喃和三乙胺在各自检测质量浓度范围内与峰面积线性关系良好（r在0.999 0~0.999 3之间）;精密度、重复性试验的RSD≤2.6%;平均加样回收率分别为95.6%、97.0%、103.2%、94.3%、98.2%（RSD在2.1%~4.9%之间,n=9）;最低检测限分别为2、2、2、0.7、0.3μg/ml。结论：该方法快速、灵敏、准确,可用于替考拉宁原料药及注射剂中有机溶剂残留量测定。OBJECTIVE：To establish a method for the content determination of chloramphenicol and salicylic acid in Acne tincture. METHODS：HPLC method was adopted with the column of Shim-pack CLC-ODS with the mobile phase of methanol-water（50 ∶ 50,V/V）at the flow rate of 0.8 ml/min. The detection wavelength was 278 nm,column temperature was 35 ℃,and the volume was 10 μl. RESULTS：The linear range was 2.0-10.0 μg/ml（r=0.999 2）for chloramphenicol and 5.0-25.0 μg/ml（r=0.999 1）for salicylic acid;the RSDs of precision,stability and repeatability tests were lower than 1%;the average recoveries chloramphenicol and salicylic acid were respectively 99.77%（RSD=0.35%,n=9） and 99.29%（RSD=0.48%,n=9）. CONCLUSIONS：The method is simple,rapid,accurate,specific,precise,and can be used for quality control of Acne tincture.

关 键 词：替考拉宁 原料药 注射剂 残留溶剂 顶空气相色谱法 

分 类 号：R927.2[医药卫生—药学]