高效液相色谱法测定化妆品中13种α-羟基酸的含量

Determination of 13 kinds of α-hydroxy acids in cosmetics by high performance liquid chromatography

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。方法去样品采用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 C_(18)(4.6mm×250mm,3μm)色谱柱上进行分离,以甲醇-0.02mol/L磷酸氢二铵溶液(pH2.68)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214nm。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>0.9998),各成分的检测下限范围在1μg/g~84μg/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0.0022%~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一羟基酸的含量测定。

Objective This paper aims to establish a method for the determination of 13 kinds ofα-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 C_(18)(4.6 mm×250 mm,3μm)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 ofα-hydroxy acids were good in corresponding concentration range(r>0.9998),and the limits detection(LOD)were in the range of 1μg/g-84μg/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 ofα-hydroxy acids were detected.The contents of theseα-hydroxy acids ranged from 0.0022%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 ofα-hydroxy acids in cosmetics.