顶空气相色谱法测定盐酸头孢吡肟中残留溶剂  

Headspace gas chromatographic analysis of residual solvents in samples of cefepime hydrochloride

作　　者：何志强[1] 

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《广东药学院学报》2005年第2期150-152,共3页Academic Journal of Guangdong College of Pharmacy

摘　　要：目的建立盐酸头孢吡肟中有机残留溶剂的测定方法.方法顶空气相色谱法.色谱条件:采用DB 624 (0.35 mm I.D×30 m×3.0 μm )6%氰丙苯基、94%甲基聚硅氧烷毛细管色谱柱;柱温:45 ℃;气化室温度:150 ℃;检测室温度:280 ℃;N2为载气;柱前压力为75 kPa;H2流速:50 mL/min;空气流速:500 mL/min.结果甲醇在159～636 μg/mL,丙酮在258-1033 μg/mL,二氯甲烷在30～122 μg/mL,四氢呋喃在148～593 μg/mL质量浓度范围均呈良好的线性关系.平均回收率(n=6)分别为100.2%,RSD=6.5%;92.5%,RSD=3.7%;102.6%,RSD=6.7%;103.7%, RSD=3.1%.结论本方法操作简便、结果准确,是控制盐酸头孢吡肟中残留溶剂的可靠方法.Objective and Method Headspace gas chromatography was used to analyze the residual solvents in the samples of cefepime hydrochloride with DB 624 capillary column (30 m×0.35 mm×0.3 μm). The operating conditions were: nitrogen as the carrier gas, 75 kPa of column inlet pressure, 45 ℃ of column temperature, 150 ℃ of flame ionization detector and 280 ℃ of injector. Results The calibration curves for methanol, acetone, dichloromethane and tetrahydrofuran were linear over the ranges of 159-636 μg/mL (r=0.9960, n=5), 258~1033 μg/mL (r=0.9990, n=5), 30~122 μg/mL (r=0.9975, n=5) and 148~593 μg/mL (r=0.9992, n=5), respectively. The average recoveries of methanol, acetone, dichloromethane and tetrahydrofuran were 100.2% (RSD=6.5%, n=6), 92.5% (RSD=3.7%, n=6), 102.6% (RSD=6.7%, n=6) and 103.7% (RSD=3.1%, n=6), respectively. Conclusion The procedure provides a simple and sensitive method for monitoring residual solvents in the samples of cefepime hydrochloride.

关 键 词：顶空气相色谱法 盐酸头孢吡肟 有机溶剂 

分 类 号：R927[医药卫生—药学]