直接进样杆在线衍生GC-MS测定阿司匹林中的水杨酸  

Determination of free salicylic acid in aspirin by gas chromatography-mass spectrometry with direct sample introduction on-line derivatization

作　　者：李祖光[1] 国明[1,2] 聂晶[1] 张小平[1] 魏丹[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310032 [2]浙江省化工研究院,浙江杭州310023

出　　处：《浙江工业大学学报》2014年第1期67-72,共6页Journal of Zhejiang University of Technology

基　　金：浙江省科技厅钱江人才计划项目(2010R10044);国家人力资源与社会保障部2011年度留学人员科技活动择优资助(优秀类)项目(2011443);浙江省本科院校中青年学科带头人学术攀登项目(Pd2013016);浙江省重点创新团队项目(2010R50018-06)

摘　　要：建立超声辅助萃取-直接进样杆在线衍生-气相色谱质谱测定阿司匹林泡腾片中游离水杨酸含量的方法.采用乙腈为提取剂进行超声萃取,以四丁基硫酸氢铵（TBAHS）为衍生化试剂进行衍生,利用直接进样杆装置在气相色谱进样口进行在线衍生以提高分析灵敏度,采用DB-5MS毛细管色谱柱,通过气相色谱-离子阱质谱进行分析测定.结果表明：水杨酸在1.0～30.0 μ g/mL范围内线性关系良好（r=0.997 8）,方法的检出限和定量限分别为0.09 μg/mL和0.28 μ g/mL.方法具有操作简单,无需净化步骤,准确度高,重现性好等优点,可适用于阿司匹林药物中游离水杨酸含量的测定.A method using sonication-assisted extraction for determining free salicylic acid in aspirin effervescent tablets was established by gas chromatography-mass spectrometry with direct sample introduction on-line derivatization.Salicylic acid in medicine samples was extracted by acetonitrile solution.The samples were stirred with tetrabutylammonium hydrogen sulfate （TBAHS） as derivatization reagent.The method used gas chromatography with ChromatoProbe device for on-line derivatization to improve sensitivity.Analysis was performed on a DB-5MS capillary column supplemented with gas chromatography-ion trap mass spectrometry.The calibration curves of the analyte revealed a good linear relationship over the ranges of 1.0～30.0 μg/mL （r=0.997 8）.The limit of detection （LOD） and limit of quantitation （LOQ） of the developed method were 0.09 μ g/mL and 0.28 μg/mL,respectively.This method has the advantages of convenient operation,no need of purification,high sensitivity,excellent accuracy and good reproducibility and is suitable for the determination of free salicylic acid in aspirin.

关 键 词：水杨酸 气相色谱-质谱(GC-MS) 在线衍生 四丁基硫酸氢铵 超声辅助萃取 

分 类 号：O657.63[理学—分析化学]