摘要
建立了采用高效液相色谱法同时测定化妆品中视黄醇、视黄醇乙酸酯、视黄醇棕榈酸酯及羟基频哪酮视黄酸酯的方法.梯度洗脱、柱温 30℃、流速 1.5 mL/min条件下,采用色谱柱 Wondasil C18 Superb(4.6 mm×250 mm,5 μm)分离,分别在 325 和 358 nm波长下检测,用高效液相色谱仪进行分析,并对提取方法、流动相等条件进行优化.结果表明:不添加四氢呋喃提取样品对含量检测结果无影响;以甲醇为提取液、甲醇-水为流动相,视黄醇、视黄醇乙酸酯和羟基频哪酮视黄酸酯 3 种化合物在 0.02～50.00 mg/L范围内线性良好,视黄醇棕榈酸酯在 0.20～50.00 mg/L范围内线性良好,相关系数(r2)>0.999;视黄醇、视黄醇乙酸酯、视黄醇棕榈酸酯和羟基频哪酮视黄酸酯的检出限分别为 0.01、0.01、0.04 和 0.01 mg/L,定量限分别为 0.02、0.02、0.10 和 0.02 mg/L;视黄醇、视黄醇乙酸酯和羟基频哪酮视黄酸酯 3 种化合物在50.00、20.00、0.02 mg/L 三个不同水平质量浓度的加标提取回收率为 89.06%～104.30%,精密度为3.45%～3.95%;视黄醇棕榈酸酯在 50.00、20.00、0.20 mg/L 三个不同水平质量浓度的加标提取回收率为 91.66%～103.25%,精密度为 3.61%～3.69%.该方法快速、简单、准确,适用于化妆品中视黄醇、视黄醇乙酸酯、视黄醇棕榈酸酯和羟基频哪酮视黄酸酯含量的测定.
Abstract
A method for the simultaneous determination of retinol,retinol acetate,retinol palmitate and hydroxypinacone retinol in cosmetics using high-performance liquid chromatography is established.With gradient elution,column temperature of 30℃and flow rate of 1.5 mL/min,a chromatographic column of Wondasil C18 Superb(4.6 mm×250 mm,5 μm)was used for separation,detection at 325 and 358 nm,and analysis was performed using high-performance liquid chromatography.The extraction method and flow conditions were optimized.The results showed that the addition of tetrahydrofuran can not affect the content detection results of extracted samples;using methanol as extraction solution and methanol/water as mobile phase,three compounds of retinol,retinol acetate and hydroxypinacone retinol have good linearity in the range of 0.02～50.00 mg/L,while retinol palmitate has good linearity in the range of 0.20～50.00 mg/L,with a correlation coefficient(r2)>0.999.The detection limits of retinol,retinol acetate,retinol palmitate and hydroxypinacone retinoate are 0.01,0.01,0.04,and 0.01 mg/L,respectively,and the quantification limits are 0.02,0.02,0.01,and 0.02 mg/L,respectively.The recovery rates of spiked extraction of retinol,retinol acetate and hydroxypinacone retinol at three different concentrations of 50.00,20.00 and 0.02 mg/L are 89.06%to 104.30%,with a precision of 3.45%to 3.95%;and the recovery rates of spiked extraction of retinol palmitate at three different concentrations of 50.00,20.00 and 0.20 mg/L are 91.66%～103.25%,with a precision of 3.61%～3.69%.This method is fast,simple and accurate so that it is suitable for the determination of retinol,retinol acetate,retinol palmitate and hydroxypinacone retinol in cosmetics.
维普
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