GC-TEA同时测定化妆品中的5种挥发性亚硝胺  

Simultaneous Determinations of Five Kinds of Volatilenitrosamines in Cosmetics by Gas Chromatography-thermal Energy Analyser

作　　者：邢昆明[1,2] 刘华 王贻坤[1,4] 朱灵[1] 刘勇[1] 王安[1] 计敏[1,4] XING Kun-ming LIU Hua WANG Yi-kun ZHU Lin LIU Yon WANG An JI-Min(Institute of Applied Technology, Hefei Institutes of Physical Sciences, Chinese Academy of Sciences, Hefei 230051, China University of Science and Technology of China, Hefei 230026, China Hefei Product Quality Supervision＆Inspection Institute, Hefei 238000, China Anhui Yikangda Photoelectric Technology Co., Ltd., Hefei 230031, China)

机构地区：[1]中国科学院合肥物质科学研究院应用技术研究所,安徽合肥230031 [2]中国科学技术大学,安徽合肥230026 [3]合肥市产品质量监督检验所,安徽合肥238000 [4]安徽易康达光电科技有限公司,安徽合肥230031

出　　处：《安徽化工》2016年第6期100-103,106,共5页Anhui Chemical Industry

基　　金：安徽省重大科学仪器专项(1510115223)

摘　　要：建立了化妆品中5种挥发性亚硝胺的气相色谱-热能分析仪联用（GC-TEA）同时分析测定方法。利用丙酮在超声条件下将5种挥发性亚硝胺从水溶性或脂溶性化妆品样品中萃取出来,经过高速冷冻离心后,用二氯甲烷分三次萃取提取上清液,收集上清液于底部加入无水硫酸钠试管中,水相在氮吹仪上浓缩后添加内标N-亚硝基二丙胺,再经微孔滤膜过滤到棕色色谱瓶进样检测。该方法能够有效地检测出化妆品中的5种挥发性亚硝胺,方法定量限为13.5~27μg/kg,回收率为86.2%~95.4%,精密度为2.0%~6.5%。本方法杂质峰少,准确度、灵敏度高,线性范围宽,能够满足化妆品中5种挥发性亚硝胺的测定要求。A comprehensive analytical method based on gas chromatography -thermal energy analyzer has been developed for simultaneous determinations of five kinds of volatile nitrosamines in Cosmetics. Five kinds of volatile nitrosamines were extracted with acetone from water-soluble or fat-soluble cosmetics sample under ultrasonic conditions. The mixed solution was layered through high speed freeze centrifugation. Then supernatant was extracted with methylene chloride three times and collected by test tube with anhydrous sodium sulfate at the bottom , the internal standard N-nitroso dipropylamine was added to it ,after the upper aqueous phase was concentrated by Nitrogen blowing instrument, and then filtered by microporous membrane to the brown chromatographic bottle for following detection. The sample was detected by gas chromatography-thermal energy analyzer （GC-TEA）. This method could effectively detect the five kinds of volatile nitrosamines in cosmetics. The limits of quantification were from 13.5 to 27μg/kg. The recovery rates were from 86.2% to 95.4%, the precisions were from 2.0 % to 6.5%. The method had small impurity peaks and wide linear range ,also was accurate and provided with high sensitivity, which was suitable for determination of five kinds of volatile nitrosamines in cosmetics.

关 键 词：气相色谱-热能分析仪 化妆品 挥发性亚硝胺 

分 类 号：O656.3[理学—分析化学]