摘要
目的建立适合头孢泊肟酯中有机残留溶剂的测定方法。方法采用Agilent DB-624毛细管柱(30.0 m×0.25 mm×1.4μm),顶空气相色谱法,FID检测器,运用外标法、内标法、标准加入法和加校正因子的标准加入法测定分析头孢泊肟酯中乙醛、甲醇、乙醇、异丙醇、二氯甲烷、异丙醚、丁酮、乙酸乙酯、四氢呋喃、环己烷、吡啶、甲苯和乙酸正丁酯的残留量。结果有效分离上述各有机溶剂,在考察的浓度范围内各方法的结果线性均良好,r值在0.9980~1.0000之间;各残留溶剂的检出限在0.0250~0.3284μg/m L之间。残留溶剂间回收率差异显著,乙醛回收率最低,为39.7644%~42.1885%,环己烷回收率最高,为125.3627%~132.2517%。结论标准加入法分析适用于头孢泊肟酯有机溶剂残留的测定。
Objective To establish a suitable method for determination of residual solvents in Cefpodoxime Proxetil.Methods Agilent DB-624 capillary column（30.0 m×0.25 mm×1.4 μm） was used, with FID detector, thirteen residual solvents（acetaldehyde, methanol, ethanol, isopropanol, dichloromethane, isopropyl ether, butanone, ethylacetate, tetrahydrofuran, cyclohexane, pyridine, toluene, butyl acetate） in Cefpodoxime Proxetil were determinated and analyzed by external standard method, internal standard method, standard addition method and correction factor standard addition method. Results The results showed that all residual solvents could be separated, and good linear relationships were obtained in their respective concentration ranges in the methods（r = 0.9980-1.0000）, the detection limits were between 0.0250 to 0.3284 μg/m L. And significant differences recovery rates between all kinds of residual solvents, with the lowest recovery rates in acetaldehyde（39.7644%-42.1885%） and with the highest recovery rates in cyclohexane（125.3627%-132.2517%）. Conclusion The standard addition method is the most suitable determination method for the residual solvents in Cefpodoxime Proxetil.
作者
张清国
周芳
郭树兴
何明
王丽敏
陈典清
ZHANG Qingguo ZHOU Fang GUO Shuxing HE Ming WANG Limin CHEN Dianqing(Fujian Gutian Pharmaceutical Co., Ltd., Fujian Province, Gutian 352200, Chin)
出处
《中国医药导报》
CAS
2017年第22期37-41,共5页
China Medical Herald
关键词
头孢泊肟酯
残留溶剂
乙醛
丁酮
乙酸乙酯
气相色谱法
Cefpodoxime Proxetil
Residual solvent
Acetaldehyde
Butanone
Ethylacetate
Gas chromatography
