化妆品中儿茶素类组分的高效液相色谱测定法  

Determination of catechins in cosmetics by high-performance liquid chromatography

作　　者：茹歌 韩晶 彭兴盛 郑荣 RU Ge;HAN Jing;PENG Xingsheng;ZHENG Rong(Shanghai Institute for Food and Drug Control,NMPA Key Laboratory for Monitoring and Evaluation of Cosmetics,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验研究院国家药品监督管理局化妆品监测评价重点实验室,上海201203

出　　处：《上海预防医学》2022年第6期601-606,共6页Shanghai Journal of Preventive Medicine

摘　　要：【目的】建立化妆品中9种儿茶素类组分表儿茶素(EC)、表儿茶素没食子酸酯(ECG)、表没食子儿茶素(EGC)、表没食子儿茶素没食子酸酯(EGCG)、没食子儿茶素(GC)、没食子儿茶素没食子酸酯(GCG)、儿茶素没食子酸酯(CG)、右旋儿茶素(CD)、没食子酸(GA)的高效液相色谱(HPLC)定量测定法。【方法】水剂、膏霜乳液、凝胶类、油类化妆品经超声提取、离心处理,上清液经0.45µm微孔滤膜过滤后,取续滤液进样,采用Kromasil 100⁃5 C18反相色谱柱(5µm,4.6 mm×250 mm)分离,以0.05%三氟乙酸水溶液-甲醇梯度洗脱,采用二级管阵列检测器(DAD)对10批市售化妆品中的9种儿茶素类组分进行定性、定量测定。【结果】HPLC检测法的相对标准偏差(RSD)为0.11%~6.30%(n=3);平均回收率为84.4%~114.7%。9种化合物在0.49~105.39 mg·L^(−1)的浓度范围内呈线性关系(r>0.995)。HPLC检测法的检出限均为5µg·g^(−1)。10批市售化妆品中3批为阳性,其紫外光谱扫描图与标准品匹配结果一致。【结论】9种儿茶素类组分的HPLC测定法高效、灵敏、准确,适用于化妆品中EC、ECG、EGC、EGCG、GC、GCG、CG、CD、GA共9种组分的检测。[Objective]To establish a high⁃performance liquid chromatography(HPLC)quantitative method for the determination of epicatechin(EC),(-)⁃epicatechin gallate(ECG),(-)⁃epigallocatechin(EGC),(-)⁃epigallocatechin gallate(EGCG),(-)⁃gallocatechin(GC),(-)⁃gallocatechin gallate(GCG),(-)⁃catechin gallate(CG),cianidanol(CD)and gallic acid(GA)in cosmetics.[Methods]Samples were prepared by ultrasonic extraction and followed by high-speed centrifugation of the extraction solution.The supernatant was filtered by 0.45µm Millipore filter.The continued filtrate was taken for analysis.A reversed phase column,Kromasil 100-5 C18(5µm,4.6 mm×250 mm)was used with 0.05%trifluoroacetic acid buffer and methanol as mobile phase under the condition of gradient elution.Diode array detection(DAD)method was used for the determination.Qualitative and quantitative determination was conducted in 10 batches of commercially available cosmetics.[Results]The relative standard deviations(RSD)were in the range of 0.11%−6.30%(n=3);the recoveries were in the range of 84.4%−114.7%.The method showed a good linearity within the concentration range of 0.49−105.39 mg·L^(−1)(r>0.995).The detection limit was 5µg·g^(−1).In 10 batches of commercially available cosmetics,three batches showed positive result,which was consistent with the UV spectrum of the standard.[Conclusion]This method is efficient,sensitive and accurate.It is applicable to the determination of EC,ECG,EGC,EGCG,GC,GCG,CG,CD and GA in cosmetics.

关 键 词：高效液相色谱法 化妆品 儿茶素 

分 类 号：R173[医药卫生—妇幼卫生保健]