摘要
目的研究建立了一种测定化妆品中游离甲醇的气相色谱分析方法。方法对水剂类、膏霜类、香波类等不同类型的化妆品样品,分别采用顶空法或直接法进行样品预处理,对发胶类化妆品样品采用蒸馏法进行处理,待测组分经HP-INNOWax(30 m×0.25 mm×0.25μm)色谱柱在75℃柱温条件下恒温8 min进行分离,采用氢火焰离子化检测器进行测定,外标法定量。结果实验结果表明,水剂类、膏霜类、香波类、发胶类等不同类型化妆品在各自线性范围内呈良好线性关系,相关系数(r2)均>0.99,以3倍和10倍信噪比估算方法的检出限及定量限分别为6 mg/kg和20 mg/kg。在20 mg/kg^2000 mg/kg范围内低、中、高3个添加水平下,样品加标回收率在92.4%~112.4%之间,相对标准偏差为1.69%~7.46%(n=6)。结论本方法简便、可靠、重现性好、灵敏度高,可为化妆品检验和生产质量控制提供科学依据和技术支持。
Objective To develop a gas chromatographic method for analysis of free methanol in cosmetics. Methods The samples of lotion, cream and shampoo were extracted by headspace or direct method, and the hairspray samples were extracted by distillation method. These cosmetics samples were then separated on HP - INNOWax chromatographic column at 75 ℃ for 8 min, and detected by hydrogen flame ionization detector and quantified with external standard method. Results Cosmetics of individual hnear range （ r 〉 0.99）. The limits of detection lotion, cream, shampoo and hairspray showed good linearity in their 2 （LODs） and the limits of qualification （LOQs） of the method were 6 mg,/kg （ S/N 〉 3 ） and 20 mg/kg （ S/N 〉 10 ）, respective- ly. The average recoveries of free methanol were 92.4% - 112.4% at three spiked levels in the range of 20 mg/kg - 2000 mg/kg, and the relative standard deviations （RSDs） were between 1.69% and 7.46% （ n = 6）. Conclusion The method was proven to be accurate, rapid, stable and highly sensitive and it can provide scientific basis and technical support for the in- spection and production quality control of cosmetics.
出处
《中国卫生检验杂志》
北大核心
2014年第6期776-778,共3页
Chinese Journal of Health Laboratory Technology
基金
质检公益性行业科研专项计划资助项目(2012104013-4)
国家标准化管理委员会计划资助项目(20101097-T-607)
