摘要
目的针对《化妆品技术规范》(2015年版)中测定化妆品中二甘醇方法的局限性,建立气相色谱法检测不同基质的化妆品(水、乳、霜、凝胶、膏)中二甘醇含量的方法。方法水状样品用甲醇超声提取后直接过滤上样,乳、霜、凝胶等样品用甲醇超声提取,离心后过滤上样,膏状样品先用无水硫酸钠研磨,甲醇超声提取,离心过滤后上样检测,采用气相色谱–氢火焰离子化检测器进行测定,基质匹配标准溶液外标法定量。结果二甘醇在1~1 000μg/mL浓度范围内线性关系良好(r=0.9997)。选取高中低3个浓度添加二甘醇标准品,乳、霜、凝胶的回收率为94.4%~95.4%,膏的回收率为85.1%~96.9%,化妆水的回收率为89.5%~98.8%,且相对标准偏差(RSD)均≤4.86%。方法检出限为0.24μg/mL,定量限为1μg/mL。结论该方法操作简单可行,测量成本低,线性范围宽,实用价值高,适用于不同基质的化妆品中二甘醇含量的检测。
Objective To develop a method for the determination of diethylene glycol in various cosmetics（emollient water, lotion, cream, gel and paste） with gas chromatography to solve limitations of detection methods used in current practice. Methods The emollient water samples were extracted with methanol by ultrasonic and detected after filtration; the lotion, cream and gel samples were extracted with methanol with ultrasonic and then centrifuged and filtered; the pastesamples were grinded with anhydrous sodium sulfate first, then extracted using ultrasonic with methanol, and finally centrifuged and filtered for detection. The diethylene glycol in the samples was determined with gas chromatography-flame ionization detector（GC-FID） and quantified with matrix-matched external standard method. Results The calibration curve presented a good linearity in the range of 1-1000 μg/mL（r = 0.999 7）. Three-level spiked recoveries were carried out using blank cosmetic extractions as substrate; the recoveries ranged from 94.4% to 95.4% for lotion, cream or gel, 85.1% to 96.9%for the paste, and 89.5% to 98.8% for emollient water; while the relative standard deviations（RSDs） were all below 4.86%.The limit of determination was 0.24 μg/mL and the limit of quantitation was 1 μg/mL. Conclusion The method is simple and easy to operate with less cost, wide linear rang, low detection linearity, and high practical value and it is suitable for the detection of diethylene glycol in different cosmetic matrixes.
作者
张铧尹
朱怀娇
曹梦思
檀笑昕
连靠奇
徐向东
康维钧
刘保军
ZHANG Hua-yin;ZHU Huai-jiao;CAO Meng-si(Hygiene Inspection Laboratory,School of Public Health,Hebei Medical University,Shijiazhuang,Hebei Province 050017,China)
出处
《中国公共卫生》
CAS
CSCD
北大核心
2018年第10期1421-1424,共4页
Chinese Journal of Public Health
基金
国家自然科学基金(81302471)
关键词
二甘醇
化妆品
气相色谱法
diethylene glycol
cosmetics
gas chromatography
