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目的:通过对测定程序的一些改进,对部分高黏度的化妆品中甲醇实现精确测定,并对检测条件进行了探讨。方法:通过称量纸盒精确称量高黏度类化妆品,将称量后样品投入盛有一定量的乙醇溶液的蒸馏瓶中蒸馏,准确收集馏分,进气相色谱分离并以火焰离子化检测器(Flame ionic detector,FID)测定。结果:样品中甲醇准确完全蒸馏出来,蒸馏瓶内壁未粘附样品,称量纸的存在有效地防止溶液的暴沸。对黏稠类化妆品的加标回收率在98.5%～105%之间,以优化后实验条件对此类化妆品进行检测结果满意。结论:改进后的测定方法有效地改善了黏稠类化妆品的测定准确性,样品检测结果的平行性和重复性较好,蒸馏后的蒸馏瓶易清洗。本实验对黏稠类化妆品的测定步骤改进可以作为实际检测分析的参考,适用于实验室常规检测黏稠类化妆品中甲醇。
OBJECTIVE: To determine precisely the methanol in some high-viscosity cosmetics through some improvement of measurement procedure, and discuss the testing conditions. Methods: Accurately weighing high-viscosity cosmetics by weighing cartons, weighing the sample into a distillation flask containing a certain amount of ethanol solution to distillate, collecting the distillate accurately, separating the gas chromatographically and using a flame ionization detector Flame ionic detector, FID). Results: The methanol in the sample was completely and accurately distilled off. The inner wall of the distillation flask did not adhere to the sample. The weighing paper effectively prevented bumping of the solution. The spiked cosmetics spiked recoveries between 98.5% to 105%, with optimized experimental conditions for the detection of such cosmetics satisfactory results. Conclusion: The improved method can effectively improve the determination of viscous cosmetics. The parallelism and repeatability of the test results are good. The distilled flask is easy to clean. In this experiment, the improvement of viscous cosmetic procedure can be used as a reference for practical testing and analysis. It is suitable for the laboratory routine testing of methanol in viscous cosmetics.