顶空气相色谱法测定盐酸头孢吡肟中残留溶剂
顶空气相色谱法,,顶空气相色谱法；盐酸头孢吡肟；有机溶剂,1实验部分,2实验结果,3讨论,参考文献
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。关键词 顶空气相色谱法；盐酸头孢吡肟；有机溶剂
Headspace gas chromatographic analysis of residual solvents in samples of cefepime hydrochloride
HE Zhiqiang
(Guangzhou Institute for Drug Control, Guangzhou 510160, China)
Abstract 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. ......
您现在查看是摘要页，全文长 6331 字符。