化妆品中10种α-羟基酸的高效液相色谱检测及质谱确证

Determination and verification of 10α-hydroxy acids in cosmetics by high performance liquid chromatography and mass spectrometry

目的建立同时测定化妆品中10种α-羟基酸(葡糖醛酸、酒石酸、羟基乙酸、苹果酸、乳酸、柠檬酸、2-羟基丁酸、扁桃酸、二苯乙醇酸、羟基辛酸)含量的高效液相色谱方法及液相色谱-串联质谱确证方法。方法色谱柱为SHISEIDO CAPCELL PAK C_(18) AQ(4.6 mm×250 mm,5μm),流动相为甲醇-0.1 mol·L^(-1)的磷酸氢二铵溶液,梯度洗脱,外标法定量;对疑似阳性样品,进一步采用液相色谱-串联质谱法进行确证,离子源为电喷雾离子源(ESI),在负离子扫描方式下,以一级和二级全扫描模式进行检测。结果10种α-羟基酸在各自浓度范围内与峰面积线性关系良好,相关系数均大于0.9995,检测限为4~329μg·g^(-1),平均回收率在94.2%~111.9%,RSD在0.30%~4.8%。采用该法对30批化妆品样品进行检验,其中1批检出羟基乙酸,2批检出乳酸,含量在0.4%~1.3%。结论本法简便、快速、准确,适用于化妆品中10种α-羟基酸测定。

Objective To simultaneously determine 10α-hydroxy acids(glucuronic acid,tartaric acid,glycolic acid,malic acid,lactic acid,citric acid,2-hydroxybutyric acid,mandelic acid,benzilic acid and hydroxycaprylic acid)in cosmetics by high performance liquid chromatography and mass spectrometry.Methods A SHISEIDO CAPCELL PAK C_(18) AQ chromatographic column(4.6 mm×250 mm,5μm)was used with gradient elution of methanol-0.1 mol·L^(-1)diammonium hydrogen phosphate solution as the mobile phases.Quantification analysis was performed by the external standard method.Suspected positive samples were further confirmed by liquid chromatography-tandem mass spectrometry.Electrospray ion source was detected in negative ion modes with full scan MS and full scan MS^(2) mode.Results Good linearity was achieved for all the 10α-hydroxy acids,and the correlation coefficients were all greater than 0.9995.The limits of detection were 4~329μg·g^(-1).The average recoveries were within 94.2%~111.9%,with RSD of 0.30%~4.8%.Totally 30 batches of cosmetics were detected,among which glycolic acid was detected in 1 batch,and lactic acid was detected in 2 batches,with the content at 0.4%~1.3%.Conclusion This method is simple,rapid and accurate for the simultaneous determination of 10α-hydroxy acids.