GC-MS法测定皮革中甲基环硅氧烷的检测方法研究  

Determination of Methylcyclosiloxane in Leather by GC-MS

作　　者：杜英英[1] 李海燕[1] 别红梅 DU Yingying;LI Haiyan;BIE Hongmei(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 201114,China)

机构地区：[1]上海市质量监督检验技术研究院,上海201114

出　　处：《皮革与化工》2022年第4期16-19,共4页Leather And Chemicals

基　　金：上海市科学技术委员会研发公共服务平台建设项目《上海市日用消费品质量安全检测专业服务平台》(项目编号:14DZ2293000)。

摘　　要：利用气质联用仪(GC-MS)建立了皮革中八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)、十二甲基环六硅氧烷(D6)等三种甲基环硅氧烷含量的检测方法。以乙酸乙酯为溶剂,45℃振荡提取60 min,GC-MS测定,外标法定量,进行了3个添加水平的7次平行试验,结果表明:添加浓度为(10~400)mg/kg时,样品中的回收率在83.5%~100.6%之间,相对标准偏差(RSD,n=7)在2.1%~6.4%之间,方法定量限在(4.7~5.4)mg/kg之间,满足分析要求。该方法适用于皮革中D4、D5和D6等甲基环硅氧烷的日常检测,对相关检测标准的制定也具有一定的指导意义。A method for simultaneous determination of methylcyclosiloxane(D4,D5 and D6)in leather by gas chromatography mass spectrography(GC-MS)was established.Samples were extracted with ethyl acetate under water bath shaking,then analyzed by GC-MS and quantified by external standard method.The average recoveries of D4,D5 and D6(10~400 mg/kg)in leather at three levels with seven times parallel test were ranged from 83.5%to 100.6%with 2.1%to 6.4%of relative standard deviations(n=7).The limit of detection of this method was(4.7~5.4)mg/kg.The method is suitable for routine analysis of methylcyclosiloxane(D4,D5 and D6)in leather,and it also has certain guiding significance to the development of relevant testing standards.

关 键 词：皮革 气质联用仪 甲基环硅氧烷 检测 八甲基环四硅氧烷(D4) 十甲基环五硅氧烷(D5) 十二甲基环六硅氧烷(D6) 

分 类 号：TS57[轻工技术与工程—皮革化学与工程]