顶空气相色谱法测定溴芬酸钠中有机溶剂残留量  

Determination of Residual Organic Solvents in Bromfenac Sodium by Headspace Gas Chromatography

作　　者：杨海霞 王长斌 邢玉仁 

机构地区：[1]山东省药学科学院,山东省化学药物重点实验室,济南250101 [2]山东福瑞达医药集团公司,山东省黏膜与皮肤给药技术重点实验室

出　　处：《中国药师》2015年第6期888-889,925,共3页China Pharmacist

基　　金："重大新药创制"科技重大专项(编号:2009ZX09301-013)

摘　　要：目的:建立顶空毛细管气相色谱法测定溴芬酸钠中有机溶剂残留量。方法:采用顶空气相色谱法,色谱柱为HP-5毛细管柱,载气为氮气,流速为0.8 ml·min-1。FID检测器,检测器温度为250℃;进样口温度为200℃;柱温采取程序升温,初始温度40℃,维持10 min,以30℃·min-1升温至150℃,维持5 min。顶空进样,顶空瓶平衡温度为100℃,平衡时间为20 min。以二甲亚砜为溶剂,外标法测定溴芬酸钠中甲苯、异丙醇、二氯甲烷、甲醇及异丙醚的残留量。结果:各组分完全分离,线性关系良好,5种溶剂的平均回收率分别为98.9%(RSD=2.01%)、99.2%(RSD=1.95%)、99.6%(RSD=1.65%)、100.5%(RSD=1.38%)、100.8%(RSD=1.36%)(n=9)。结论:该法简便、准确,可用于溴芬酸钠中5种有机溶剂残留量的测定。Objective： To establish a headspace capillary GC method for the determination of residual solvents in bromfenac sodium. Methods： A headspace GC was used to separate the residual solvents on an HP-5 capillary column with an FID detector. The carrier gas was nitrogen at the flow rate of 0.8 ml·min^-1. The temperature of the injector was 200 ℃ and that of the FID was 250 ℃. The programmed column temperature was set as follows： maintained at 40 ℃ for 10 min, and then raised to 150 ℃ at the rate of 30 ℃ ·min^-1 and maintained for 5 min. The containers of headspace injector were in equilibrium at 100 ℃ for 20 min. Dimethyl sulfoxide was used as the solvent. The amount of the residual solvents, such as methylbenzene, isopropanol, dichloromethane, methanol and iso- propyl ether was calculated by an external standard method. Results： All the solvents could be completely separated with good linear relationship. The average recovery of the five solvents was 98.9% （ RSD = 2.01% ）, 99.2% （ RSD = 1.95% ）, 99.6% （ RSD = 1.65% ）, 100.5% （ RSD = 1.38% ） and 100.8% （ RSD = 1.36% ） （ n = 9）, respectively. Conclusion： The method is simple and accurate in the determination of the five residual solvents in bromfenac sodium.

关 键 词：溴芬酸钠 有机溶剂残留 顶空气相色谱法 

分 类 号：TQ460.72[医药卫生—药物分析学]