目的 建立化妆品中13种α-羟基酸的高效液相色谱检测方法.方法 样品采用10％甲醇超声提取葡糖醛酸、葡萄糖酸、酒石酸、羟基乙酸、丙酮酸、苹果酸、乳酸、柠檬酸、2-羟基丁酸9个水溶性成分,采用甲醇超声提取扁桃酸、二苯乙醇酸、羟基辛酸、2-羟基癸酸4个脂溶性成分,在ChromCore AQ C18(4.6 mm × 250 mm,3 μm)色谱柱上进行分离,以甲醇-0.02mol/L磷酸氢二铵溶液(pH 2.68)为流动相,梯度洗脱,流速为0.7ml/min,进样量:5μl,柱温:25 ℃,二极管阵列检测器检测,检测波长为214 nm.结果 13种α-羟基酸在考察的质量浓度范围内呈良好的线性关系(r＞0.999 8),各成分的检测下限范围在1 μg/g～84 μg/g,3个浓度水平的平均加标回收率为82.6％～111.9％,RSD范围为0.2％～4.3％.应用该方法对70批化妆品进行检测,结果检出5种α-羟基酸,α-羟基酸总量在0.002 2％～5.18％,均未超过《化妆品安全技术规范》(2015版)规定的最大允许浓度6％.结论 本方法具有可操作性强、重复性好、灵敏度高等特点,可用于化妆品中13种α-羟基酸的含量测定.
Determination of 13 kinds of α-hydroxy acids in cosmetics by high performance liquid chromatography
Objective This paper aims to establish a method for the determination of 13 kinds of α-hydroxy acids in cosmetics by high performance liquid chromatography(HPLC).Methods The samples were ultrasonically extracted by 10％methanol solution for 9 water-soluble components of glucuronic acid,gluconic acid,tartaric acid,glycolic acid,pyruvate,malic acid,lactic acid,citric acid,and 2-hydroxybutyric acid.Four fat soluble components of mandelic acid,diphenylglycolic acid,hydroxycaprylic acid and 2-hydroxycaprylic acid were extracted by methanol ultrasonography.The separation was performed on a ChromCore AQ C18(4.6 mm ×250 mm,3 μm)column with the mobile phase of methanol-0.02 mol/L diammonium hydro-gen phosphate solution(pH=2.68)in gradient elution.The flow rate was 0.7 ml/min,the column temperature was 25 ℃.The detection wavelength was set at 214 nm with a diode array detector.Results The linear range of 13 kinds of α-hydroxy acids were good in corresponding concentration range(r＞0.999 8),and the limits detection(LOD)were in the range of 1 μg/g-84 μg/g.The average recoveries of three different concentration levels were within 82.6％-111.9％,with the RSD of 0.2％-4.3％.The method was used to determine 70 batches of cosmetics.The results showed that 5 kinds of α-hydroxy acids were detected.The contents of these α-hydroxy acids ranged from 0.002 2％to 5.18％,which did not exceed the maxi-mum allowable concentration(6％)in Safety and Technical Standards for Cosmetics(2015 edition).Conclusion The method has the characteristics of good operability,reproducibility and high sensitivity,and it can be used to determine 13 kinds of α-hydroxy acids in cosmetics.
High performance liquid chromatographyα-hydroxy acidsGluconic acidPyruvic acid2-hydroxydecanoic acidCosmeticsContent determination
NETL
NSTL
万方数据
维普
