格隆溴铵起始物料3-羟基-1-甲基四氢吡咯异构体的分析  

Analysis of the isomers of 1-methyl-3-pyrrolidinol

作　　者：于洋 赵悦新 陶闰红 赵春杰[2] YU Yang;ZHAO Yuexin;TAO Runhong;ZHAO Chunjie(Liaoning Pharma-Union Pharmaceutical Co.Ltd.,Benxi 117004,China;School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]辽宁药联制药有限公司,辽宁本溪117004 [2]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2018年第10期857-859,864,共4页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立高效液相色谱法对格隆溴铵起始物料3-羟基^(-1)-甲基四氢吡咯异构体进行检验。方法以直链淀粉-3-氯苯基氨基甲酸酯键合型硅胶柱为固定相,正己烷-无水乙醇-三乙胺(体积比97∶3∶0. 5)为流动相,柱温为35℃,流速为1. 0 mL·min^(-1),检测器为示差折光检测器,检测器温度为40℃。结果 3-羟基^(-1)-甲基四氢吡咯异构体能达到良好分离。供试品溶液中两个异构体峰与R型、S型对照溶液中色谱峰的出峰时间一致,专属性良好; R型、S型检测限均为30. 47 mg·L^(-1); 4 h内供试品溶液稳定性良好;流速在(1. 0±0. 05) mL·min^(-1)、柱温在(35±5)℃内耐用性良好。结论所建立的分析方法适用于格隆溴铵起始物料3-羟基^(-1)-甲基四氢吡咯异构体的质量控制稳定性监测。Objective To establish a high performance liquid chromatography method to separate the isomers of 1-methyl-3-pyrrolidinol. Methods An amylose-3-chlorophenylcarbamate bonded silica gel column was used as stationary phase and the column tempreture was 35 ℃. The mobile phase was consisted of N-hexaneanhydrous ethanol-trimethylamine（ V∶ V∶ V = 97∶ 3∶ 0. 5 at a flowrate of 1. 0 mL·min^-1. The temperature of the refractive index detector was 40 ℃. Results The isomers could be well separated by the improvement of the separation conditions. The retention time of the two isomers in the test solution was consistent with that of the position solution R and S,demonstrating that the specificity was good. The limit of detection was determined when the concentration of both of the isomers were 30. 47 mg·L^-1. The stability of the test solution was good within 4 h. The durability. was good at a flowrate of（ 1. 0 ± 0. 05） mL·min^-1 and a tempreture of（ 35 ± 5） ℃. Conclusion The method is found to be simple operation and high durability,can control the product release detection and stability monitoring effectively.

关 键 词：高效液相色谱法 直链淀粉-3-氯苯基氨基甲酸酯键合型硅胶柱 异构体分离 

分 类 号：R917[医药卫生—药物分析学]