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HPLC法同时测定化妆品中3-O-乙基抗坏血酸和抗坏血酸棕榈酸酯
杨云, 郭长虹, 李鑫宇
广州质量监督检测研究院 国家化妆品质量监督检验中心
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,5 μ m)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10.0 mg/kg;抗坏血酸棕榈酸酯在2~200 mg/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。
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
DOI:10.13222/j.cnki.dc.2017.01.007
分类号:
基金项目:
Simultaneous determination of 3-O-ethyl-ascorbic acid and ascorbyl palmitate in cosmetics by HPLC
YANG Yun, GUO Chang-hong, LI Xin-yu
National Center for Quality Supervision and Testing of Cosmetics (Guangzhou), Guangzhou Quality Supervision and Testing Institute
Abstract:
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 C 18 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 1~100 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 2~200 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.
Key words:  cosmetics  3-O-ethyl-ascorbic acid  ascorbyl palmitate  high performance liquid chromatography(HPLC)  simultaneous determination

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