摘要
目的建立帕瑞昔布钠起始原料5-甲基-3,4-二苯基异噁唑中残留溶剂的测定方法。方法采用顶空进样毛细管气相色谱法。色谱柱:Agilent HP-INNOWAX毛细管柱(60 m×0.32 mm×0.5μm);程序升温;检测器:FID,温度250℃;恒定柱流量3.5 mL·min^(-1);载气:高纯氮气。结果在该色谱条件下,甲醇、异丙醇、乙酸乙酯和四氢呋喃达到完全分离,线性相关系数均大于0.9999,平均回收率均在93.5%~102.5%(RSD均小于2.0%,n=3)。结论建立的方法操作简便,灵敏度高,结果准确,可有效检测帕瑞昔布钠起始原料中有机溶剂的残留量。
Objective To establish a headspace gas chromatography method to determine the residual solvents in parecoxib sodium starting material. Methods Headspace capillary gas chromatography was used. The determination was performed on an HP-INNOWAX capillary column by temperature programming. The temperature of flame ionization detector was set at 250℃. Steady flow was set at 3.5 mL · min ^- 1. High purity N2 was used as the carrier gas. Results Methanol, isopropyl alcohol, tetrahydrofuran and ethyl acetate were completely separated in optimal chromatographic condition. Good linearities were obtained with all correlation coefficients more than 0.9999. The average recoveries were 93.5% -- 102.5% and the relative standard deviations of recoveries （n = 3） were lower than 2.0%. Conclusion The established method is simple, sensitive and accurate. It can be effectively used in the determination of residual solvents in parecoxib sodium starting material.
出处
《中南药学》
CAS
2018年第2期216-220,共5页
Central South Pharmacy
关键词
帕瑞昔布钠起始原料
顶空气相色谱法
残留溶剂
甲醇
异丙醇
四氢呋喃
乙酸乙酯
parecoxib sodium starting material
headspace gas chromatography
residual solvent
methanol
isopropyl alcohol
tetrahydrofuran
ethyl acetate
