摘要
建立了同时测定化妆品中3-O-乙基抗坏血酸和抗坏血酸棕榈酸酯的分析方法。样品用甲醇提取剂提取后经反相C_(18)柱(4.6×250 mm,5μm)分离,采用0.05%磷酸-乙腈作为流动相,梯度洗脱,流速为1.0 mL/min,二极管阵列检测器进行检测,检测波长为245 nm和240 nm,外标法定量。在优化的实验条件下,3-O-乙基抗坏血酸在1~100 mg/L线性关系良好,在空白样品中添加10、50、100 mg/kg 3个浓度水平时,得到的回收率为95%~103%,相对标准偏差为3.1%~5.9%。方法的检出限(S/N=3)为3.0 mg/kg,定量限(S/N=10)为10.0mg/kg;抗坏血酸棕榈酸酯在2~200mg/L线性关系良好,在空白样品中添加20、100、200 mg/kg 3个浓度水平时,得到的回收率为98%~104%,相对标准偏差为2.7%~4.6%。方法的检出限(S/N=3)为6.0 mg/kg,定量限(S/N=10)为20.0 mg/kg。
An analytical method for determination of 3-O-ethyl-ascorbic acid and ascorbyl palmitate in cosmetics was established.The sample was extracted with methanol extraction agent and separated by a RP C18 chromatographic column（4.6×250 mm,5 μm） at a flow rate of 1.0 mL/min.0.05%phosphoric acid solution-acetonitrile was used as mobile phase.The detection of 3-O-ethyl-ascorbic acid and ascorbyl palmitate were performed at detection wave length of 245 nm and 240 nm,respectively,by using high performance liquid chromatography-diode array detector（HPLC-DAD）.The external standard method was employed for quantitative analysis.Under the optimized condition,the calibration curve of 3-O-ethyl-ascorbic acid was linear in the range of 1100 mg/L.The average recoveries at three spiked levels of 10,50,100 mg/kg were between 95%and 103%,with relative standard deviation of 3.1%5.9%.The limit of detection（LOD,S/N=3） was 3.0 mg/kg and the limit of quantitation（LOQ,S/N=10） was 10.0 mg/kg.The calibration curve of ascorbyl palmitate was linear in the range of 2200 mg/L.The average recoveries at three spiked levels of 20,100,200 mg/kg were between 98%and 104%,with relative standard deviation of 2.7%4.6%.The LOD（S/N=3） was 6.0 mg/kg and the LOQ（S/N=10） was 20.0 mg/kg.
作者
杨云
郭长虹
李鑫宇
YANG Yun GUO Chang-hong LI Xin-yu(National Center for Quality Supervision and Testing of Cosmetics （Guangzhou）, Guangzhou Quality Supervision and Testing Institute, Guangzhou, Guangdong 511447, China)
出处
《日用化学品科学》
CAS
2017年第1期31-34,共4页
Detergent & Cosmetics
关键词
化妆品
3-O-乙基抗坏血酸
抗坏血酸棕榈酸酯
高效液相色谱法
同时测定
cosmetics
3-O-ethyl-ascorbic acid
ascorbyl palmitate
high performance liquid chromatography（HPLC）
simultaneous determination
