顶空毛细管气相色谱法测定盐酸普拉克索原料药中有机溶剂残留量  

Quantitative determination of organic solvent residue in crude drug of pramipexole dihydrochloride by headspace-capillary gas chromatography

作　　者：李景 赵娟芝 黄斌[2] 王诗红[2] LI Jing;ZHAO Juan-zhi;HUANG Bin;WANG Shi-hong(The Fifth Affiliated Hospital of Sun Yat-SenUniversity, Zhuhai Guangdong 519000;The Fifth Affiliated Hospital of Zunyi Medical College, ZhuhaiGuangdong 519000)

机构地区：[1]中山大学附属第五医院,广东珠海519000 [2]遵义医学院第五附属(珠海)医院,广东珠海519000

出　　处：《中南药学》2018年第11期1608-1611,共4页Central South Pharmacy

基　　金：贵州省科学技术基金项目(黔科合LH字[2014]7560号)

摘　　要：目的建立毛细管气相色谱法测定盐酸普拉克索原料药中有机溶剂残留量。方法色谱柱为DB-624毛细管柱(6%氰丙基苯基-4%二甲基聚氧硅烷为固定液,60 m×0.53 mm×3μm),载气为氮气,检测器为氢火焰离子化检测器(FID),程序升温,测定盐酸普拉克索中甲醇、乙醇、丙酮的溶剂残留量。结果在优化的柱压和顶空平衡温度色谱条件下,3种有机溶剂甲醇、乙醇、丙酮色谱峰均能得到有效分离,且质量浓度分别在2.854～428.1、4.912～736.0、4.821～723.2μg·mL^(-1)内与峰面积呈良好线性关系,回收试验符合检测要求。检测到盐酸普拉克索原料药中的残留溶剂有乙醇和丙酮,甲醇未检出。结论该方法灵敏、准确,适用于盐酸普拉克索原料药质量控制中的有机残留溶剂检查。Objective To establish a headspace-capillary gas chromatography(GC) method to determine the organic solvent residue in pramipexole dihydrochloride.Methods DB-624 capillary(60 m×0.53 mm×3 μm) column was adopted, and nitrogen was used as the carrier gas.Methanol, ethanol, and acetone were completely separated through gradient temperature method with a flame ionization detector.Results The organic solvents were effectively separated in the optimal condition.The linearity was good when the concentration of methanol, ethanol, and acetone was at 2.854-428.1 μg·mL^-1(r=0.9999), 4.912-736.0 μg·mL^-1(r=0.9999), and 4.821-723.2 μg·mL^-1(r=0.9991) respectively.The solvent residue of ethanol and acetone was detected in the sample of pramipexole hydrochloride, while that of methanol was not detected.Conclusion This method is sensitive and accurate, which can be used for the analysis of organic solvent residue in pramipexole dihydrochloride.

关 键 词：有机溶剂残留量 气相色谱法 盐酸普拉克索 

分 类 号：R927[医药卫生—药学]