顶空气相色谱法测定酒石酸罗格列酮原料药中4种有机溶剂残留量  

Determination of 4 Residual Organic Solvents in Rosiglitazone Tartrate Drug Substance by Headspace GC

作　　者：朱永琴[1] 王志远[2] 杨东菁[3] 王雪芹[1] 

机构地区：[1]河南省食品药品检验所,郑州450003 [2]河南大学药学院,河南开封475001 [3]河南大学医学院,河南开封475001

出　　处：《中国药房》2014年第37期3518-3520,共3页China Pharmacy

摘　　要：目的：建立测定酒石酸罗格列酮原料药中4种有机溶剂即甲醇、乙醇、甲苯和N，N-二甲基甲酰胺（DMF）残留量的方法。方法：采用顶空进样毛细管气相色谱法，以二甲基亚砜为溶剂，色谱柱为INNOWAX毛细管柱，载气为氮气，氢火焰离子化检测器，程序升温；顶空瓶平衡温度为80℃，平衡时间为30min。结果：4种有机溶剂均达到了完全分离；甲醇、乙醇、甲苯、DMF的检测质量浓度线性范围分别为14．72-294．4、24．8-496．0、4．51～90．2、4．62-92．4gg／ml（r为0．9991～0．9995）；平均回收率分别为97．89％、99．81％、100．55％、101．06％，RSD分别为1．19％、1．74％、0．84％、1．09％（n=3）；检测限分别为2．944、4．960、0．902、0．924μg／ml。样品中只检出了乙醇，均为O．2％。结论：建立的顶空气相色谱法测定4种有机溶剂残留量，操作简便、结果准确可靠。OBJECTIVE： To establish a method for the determination of 4 residual organic solvents as methanol, ethanol, toluene, N, N-dimethylformamide （DMF） in rosiglitazone tartrate drug substance. METHODS： Headspace gas chromatography was adopted. The determination was performed on INNOWAX capillary column with FID detector using nitrogen as carrier gas and dimethyl sulfoxide as solvent by temperature programming. The vial equilibrium temperature was 80 ℃ and equilibrium time was 30 vain. RESULTS： The 4 residual organic solvents were separated completely. The linear range were 14.72-294.4 μg/ml for methanol, 24.8-496.0 μg/ml for ethanol, 4.51-90.2 μg/ml for toluene and 4.62-92.4 μg/ml for DMF （r=0.999 1-0.999 5） ; their average recovery rates were 97.89% （RSD=1.19% , n=3） , 99.81% （RSD=1.74% , n=3） , 100.55% （RSD=0.84% , n：3） and 101.06% （RSD：l.09%, n：3）, respectively. The detection limits were 2.944, 4.960, 0.902 and 0.924 μg/ml, respectively. Only ethanol was detected in sample and its content was 0.2% usually. CONCLUSIONS： Headspace gas chromatography method is simple, accurate and reliable for the determination of 4 residual solvents.

关 键 词：顶空气相色谱法 酒石酸罗格列酮原料药 有机溶剂 残留量测定 

分 类 号：R927.2[医药卫生—药学]