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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 establish a gas chromatographic method for the determination of free methanol in cosmetics. Methods Different types of cosmetic samples, such as liquid, cream and shampoo, were pretreated by headspace method or direct method respectively. The hair styling cosmetic samples were treated by distillation. The tested components were separated by HP- INNOWax (30 m × 0.25 mm × 0.25 μm) column was heated at 75 ℃ for 8 min at room temperature. The separation was carried out by using hydrogen flame ionization detector and quantified by external standard method. Results The experimental results showed that there was a good linear relationship between the different types of cosmetics such as liquid, cream, shampoo and hair gel in their respective linear ranges with the correlation coefficients (r2)> 0.99, with 3 times and 10 times the signal to noise ratio The limit of detection and the limit of quantitation of the estimation method are 6 mg / kg and 20 mg / kg, respectively. The spiked recoveries of spiked samples ranged from 92.4% to 112.4% with relative standard deviations of 1.69% -7.46% (n = 6) at low, medium and high levels of 20 mg / kg to 2000 mg / ). Conclusion The method is simple, reliable, reproducible and sensitive. It can provide scientific basis and technical support for cosmetics inspection and production quality control.