顶空气相色谱法测定替卡西林钠原料药中残留溶剂  

Determination of residual solvents in bulk drug of ticarcillin disodium by headspace gas chromatography

作　　者：宋瑞芝 邢军[2] 常恩慧 袁敏 黄秀芬 

机构地区：[1]山东鲁抗医药股份有限公司,山东济宁272021 [2]济宁市药品检验所,山东济宁272020

出　　处：《齐鲁药事》2012年第11期644-645,共2页qilu pharmaceutical affairs

摘　　要：目的建立替卡西林钠中4种有机溶剂残留量的分离测定方法。方法采用顶空进样毛细管气相色谱法,Elite-5毛细管柱,载气为氮气,FID检测器,水为溶解介质,二氯乙烷为内标物,检测了替卡西林钠原料药中乙醇、乙腈、乙酸乙酯、四氢呋喃的残留量。结果四种残留溶剂完全分离,在所考察的浓度范围内具有良好的线性(r:0.995 3～0.995 9),乙醇、乙腈、乙酸乙酯、四氢呋喃的检测限分别为0.19,0.08,0.01,0.03μg,精密度RSD均小于5%,平均回收率为100.7%～102.7%。结论本试验建立的色谱方法简便、灵敏度高,结果准确、重现性好,适用于替卡西林钠原料药中乙醇、乙腈、乙酸乙酯、四氢呋喃残留量的检测。Objective To establish a method for the determination of four residual solvents in ticarcillin disodium. Methods The residue levels of ethanol, acetonitrile, ethyl acetate and tetrahydrofuran in bulk drug of ticareillin disodium were determined by headspaee gas chromatography with Elite -5 apillary column, nitrogen as carrier gas, FID detector, water as solvent media and dichloroethane as inside standard. Results Four residual solvents were completely separated and had good linear relationships （ r ：0. 995 3 - 0. 995 9 ）. The detection limits of ethanol, acetonitrile, ethyl acetate, tetrahydrofuran were 0.19,0.08,0.01,0.03 t^g, respectively. The RSDs of precision were less than 5 % and the average recoveries were 100.7% - 102.7%. Conclusion The method was simple, sensitive, accurate and reproducible ,it can be used for the determination of four residual solvents in bulk drug of Ticarcillin disodium.

关 键 词：顶空毛细管气相色谱法 替卡西林钠 残留溶剂 

分 类 号：R927.11[医药卫生—药学]