气相色谱法测定辛伐他汀中5种有机溶剂残留量  

Capillary Gas Chromatographic Determination of Five Residual Organic Volatile Solvents in Simvastatin

作　　者：屈颖[1] 华莲[1] 王丽琴[1] 孙长海[2] 

机构地区：[1]天津市药品检验所,天津300070 [2]天津红日药业股份有限公司,天津301700

出　　处：《药物分析杂志》2002年第6期468-470,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:测定辛伐他汀中残留有机溶剂甲醇、乙醇、环己烷、甲苯和N,N-二甲基甲酰胺的含量。方法:采用气相色谱法,氢火焰离子化检测器(FID),以二甲基亚砜为溶剂,正丙醇为内标,采用石英毛细管柱DB-624(0.32 mm×30m,1.8μm),以6％氰丙基苯-94％二甲基硅氧烷为固定相,柱温115℃维持8 min,以30℃·min^(-1)的速率升温至180℃,维持4min,气化室温度:200℃;检测器温度:240℃(FID);载气:氮气;分流比:1:60;柱前压:30 kPa;尾吹:50 mL·min^(-1);灵敏度:1;衰减4。实现了各组分的基线分离。结果:3批样品中5种有机溶剂残留量均符合要求。结论:经方法学试验验证,该方法灵敏、准确、可靠,适用于本品有机溶剂残留量的测定。Objective:To determine the contents of residual volatile organic solvents: methanol, ethanol, cyclo-hexane, toluene, N, N - dimethylformamide in simvastatin. Methods: Sample was dissolved in dimethyl sulfox-ide, 1 μL the solution was injected on a DB -624 (6% cyanopropylphenyl -94% dimethyl polysiloxane) sillica capillary column, using nitrogen as the carrier gas, split ratio: 1: 60, the column inlet pressure; 30 kPa, make -up gas: 50 mL· min-1, range: 1, attenuation: 4. The intial temperature was kept at 115℃ for 8 min, then the temperature was raised to 180 ℃ at the rate of 30 ℃· min-1 , and subsequently sustained for 4 min. The injection port and detector temperatures were 200℃ and 240℃ respectively. Under the above conditions, methanol, ethanol, cyclohexane, toluene, N, N - dimethylformamide and internal standard n- propanol were separated completely. Results: The contents of five residual volatile organic solvents in three bathes of samples were complied with the specification requirements. Conclusion: After validation, the method was proved to be accurate, sensitive and reliable. It is suitable to be adopted in the analysis of the tested solvents.

关 键 词：有机溶剂 残留量 气相色谱法 辛伐他汀 甲醇 乙醇 环己烷 甲苯 N N-二甲基甲酰胺 药品质量检验 

分 类 号：R927.11[医药卫生—药学] R972.6