GC/MS法同时分析液体制剂及口服液型保健品中31种防腐剂和抗氧化剂  

Simultaneous Determination of 31 Preservatives and Antioxidants in Liquid Preparation and Healthcare Dietetic Liquid by GC/MS

作　　者：陈安东[1] 吴兆伟[1] 余倩[1] 王铁松[1] 车宝泉[1] 丛骆骆 

机构地区：[1]北京市药品检验所,北京100035 [2]北京市食品药品监督管理局,北京100053

出　　处：《质谱学报》2014年第5期438-446,共9页Journal of Chinese Mass Spectrometry Society

基　　金：北京市科技计划项目(Z111100074211021)资助

摘　　要：为满足药品监管需要,建立了气相色谱-质谱（GC/MS）联用方法测定以水、醇等液体为基质的药品及保健品中的防腐剂和抗氧化剂。采用选择离子监测（SIM）技术,同时检测滴眼液、注射液、滴剂、涂剂、口服液型保健品中的三氯叔丁胺、苯酚、苯甲醇、山梨酸、苯甲酸、2-甲基异噻唑啉酮、脱氢乙酸、乙氧基喹啉、己基间苯二酚、对羟基苯甲酸酯等28种防腐剂及TBHQ、BHA、BHT等3种抗氧化剂。结果显示,31种物质在0.005~1mg/L范围内具有较好的线性关系,线性相关系数为0.998 5~0.999 9;在0.02~0.30mg/L加标范围内,回收率为73.6%~109.9%,相对标准偏差（RSDs）为1.2%~13.6%;检出限（LODs,S/N≥3）为0.001~0.008mg/L,定量下限（LOQs,S/N≥10）为0.003~0.020mg/L。应用该方法进行了多个批次的实际样品分析,结果表明,此方法灵敏、准确、稳定、可靠,且应用范围广泛。In order to meet the need of drug supervision, an analytical method was developed to determine the preservatives and antioxidants of medicines and healthcare dietetic liquid in the matrix of water, alcohol and other liquid by gas chromatography-mass spectrometry （GC/MS）. Selected ion monitoring （SIM） technology was used in this method. 28 preserv- atives, including acetonchloroform hemihydrate, phenol, benzyl alcohol, sorbic acid, benzoic acid, methylisothiazolinone, dehydroacetic acid, ethoxyquin, hexyl resorcinol, parabens etc, and 3 antioxidants, including TBHQ, BHA, BHT, which were used in eyedrops, injection, drops, paint, and healthcare dietetic liquid, were able to be determined by this method simultaneously. Good linearity is obtained in the range of 0. 005--1 mg/L with the correlation coefficients of 0. 998 5--0. 999 9. The mean recoveries of all the preservatives in the range of 0.02--0.30 mg/L are between 73.6% and 109.9%, and the relative standard deiations are between 1.2% and 13.6%. The limits of detection（LODs） are in the range of 0. 001--0. 008 mg/L, and the limits of quantification（LOQs）are in the range of 0. 003--0. 020 mg/L. The method is used in the analysis of multiple batches of sample. The result indicates that it is sensitive, accurate, stable, reliable and widely usable.

关 键 词：气相色谱-质谱联用(GC/MS) 防腐剂 抗氧化剂 液体制剂 注射液 保健品 口服液 

分 类 号：O657.63[理学—分析化学]