无衍生化-气相色谱-质谱联用法测定药用溴化丁基胶塞中硬脂酸和软脂酸的可提取量和迁移量  

Determination of extractable amount and migration amount of stearic acid and palmitic acid in medicinal brominated butyl rubber plug by non-derivative GC-MS

作　　者：余秋玲 张清 陆嘉莉 邱月 张永梅 陈豪 YU Qiuling;ZHANG Qing;LU Jiali;QIU Yue;ZHANG Yongmei;CHEN Hao(Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123)

机构地区：[1]重庆市计量质量检测研究院,重庆401123

出　　处：《分析试验室》2021年第4期469-473,共5页Chinese Journal of Analysis Laboratory

基　　金：重庆市市场监督管理局项目(CQSJKJ2019006)资助。

摘　　要：建立了无衍生化-气相色谱-质谱联用法定药用溴化丁基胶塞中硬脂酸和软脂酸的可提取量和迁移量的分析方法。胶塞以二氯甲烷为提取溶剂,40℃超声提取40 min,浓缩后测定可提取量。注射用冻干粉药品经复溶后用乙酸乙酯萃取,取上清液测定迁移量。采用SH-Stabilwax-DA色谱柱对目标物进行分离,外标法定量。结果表明,硬脂酸和软脂酸质量浓度在0.03~5.0 mg/L范围内线性关系良好,检出限分别为20μg/L和10μg/L,平均回收率为75.2%~118.7%,相对标准偏差为3.0%~5.9%。该方法可用于药品与包材相容性实验中硬脂酸和软脂酸的检测。A non-derivative GC-MS method for determining the extractable amount and migration amount of stearic acid and palmitic acid in medicinal brominated butyl rubber plug was established.The rubber plug was extracted with ultrasonic at 40℃for 40 min using dichloromethane as the extraction solvent,and the extracted amount was determined after concentration.The lyophilized powder for injection was redissolved,and then extracted with ethyl acetate.The supernatant was taken to determine the migration amount.The target compounds were separated by SH-Stabilwax-DA column and quantified by external standard method.Stearic acid and palmitic acid presented satisfactory linear relationships in the range of 0.03-5.0 mg/L,and the detection limits were 20μg/L and 10μg/L,respectively.The average recoveries ranged from 75.2%to 118.7%,and the RSDs were between 3.0%and 5.9%.The method can be employed for the detection of stearic acid and palmitic acid in the compatibility test between drugs and packaging materials.

关 键 词：无衍生化 气相色谱质谱联用法 硬脂酸 软脂酸 药品与包材相容性 

分 类 号：O657.63[理学—分析化学] R917[理学—化学]