气相色谱法测定格隆溴铵起始原料α-环戊基-α-苯基-α-羟基乙酸甲酯的残留溶剂  

Determination of Residual Solvents of α-cyclopentyl-α-phenyl-α-methyl glycolate from Starting Material of Glycopyrronium Bromide by Gas Chromatography

作　　者：曾少群 黄灿中 谢春燕 蔡文坚 李庆 王琴 岳峰 Zeng Shaoqun;Huang Canzhong;Xie Chunyan;Cai Wenjian;Li Qing;Wang Qin;Yue Feng(Guangdong Jiabo Phamaceutical Co.,Ltd.,Qingyuan 511517,China)

机构地区：[1]广东嘉博制药有限公司,广东清远511517

出　　处：《广东化工》2020年第10期141-144,共4页Guangdong Chemical Industry

基　　金：科技型中小企业技术创新项目《格隆溴铵注射液的药代动力学以及验证性临床研究》,项目编号(DZXQY064)。

摘　　要：目的建立气相色谱法测定格隆溴铵起始原料α-环戊基-α-苯基-α-羟基乙酸甲酯的残留溶剂。方法以N,N-二甲基甲酰胺(DMF)为溶剂,采用KB-624毛细管色谱柱(30 m×0.53 mm,3μm);氢火焰离子化检测器(FID);载气:氮气;进样口温度:200℃;检测器温度:250℃;程序升温:起始柱温35℃,保持6 min,以20℃·min-1的速率升至160℃,保持7.75 min;分流比为5︰1;进样量1μL。结果甲醇、乙醚、溴乙烷、苯乙烯均能有效分离,分别在0.0800~0.3200、0.1315~0.5260、0.0032~0.0130、0.0027~0.0111mg·m L^-1浓度范围内线性良好(R>0.999),平均回收率为96.5%~99.4%。结论该方法简便、准确,适用于α-环戊基-α-苯基-α-羟基乙酸甲酯中残留溶剂的测定,可为其质量控制提供科学依据。Objective To establish a gas chromatography method for the determination of residual solvents of α-cyclopentyl-α-phenyl-α-methyl glycolate from the starting material of glycopyrronium bromide. Methods Using N,N-dimethylformamide(DMF) as solvent and the residual solvent were separated on KB-624 capillary column(30 m×0.53 mm, 3 μm) with a hydrogen flame ionization detector(FID). Nitrogen was used as carrier gas. The injector temperature and the detector temperature was set at 200 ℃ and 250℃, respectively. The column temperature was raised from 35 ℃(kept for 6 min) to 160 ℃(then kept for 7.75 min) by program at the rate of 20 ℃·min-1;The injection volume was 1 μL with 3:1 as split ratio. Results The methanol, ether, bromoethane and styrene were separated effectively, with good linear relationships in the range of 0.0800~0.3200, 0.1315~0.5260, 0.0032~0.0130 and 0.0027~0.0111 mg·mL^-1, respectively(R>0.999), and the average recoveries ranged from 96.5 to 99.4 %. Conclusion The method is simple and accurate, which is suitable for the determination of residual solvents in α-cyclopentyl-α-phenyl-α-methyl glycolate, and can simultaneously provide scientific basic for the quality control.

关 键 词：α-环戊基-α-苯基-α-羟基乙酸甲酯 残留溶剂 气相色谱法 格隆溴铵 

分 类 号：TQ460.64[化学工程—制药化工]