超高效液相色谱-串联质谱法测定化妆品中13种α-羟基酸  

Determination ofα-hydroxy acids in cosmetics by UHPLC-MS/MS

作　　者：茹歌 许勇 韩晶 张凯 彭兴盛 郑荣 RU Ge;XU Yong;HAN Jing;ZHANG Kai;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》2024年第4期399-408,共10页Shanghai Journal of Preventive Medicine

摘　　要：【目的】建立化妆品中葡糖醛酸、酒石酸、羟基乙酸、苹果酸、乳酸、柠檬酸、2-羟基丁酸钠、扁桃酸、二苯乙醇酸、羟基辛酸、乳糖酸、葡糖酸、N-乙酰神经氨酸等13种α-羟基酸类化合物的超高效液相色谱-串联质谱(UHPLC-MS/MS)测定法。【方法】水剂、膏霜、乳液类化妆品经超声提取、澄清剂净化、10 000.0 r·min^(-1)高速离心处理,上层溶液经0.22μm微孔滤膜过滤后进样。采用Poroshell 120 EC-C18反相色谱柱(2.7μm,4.6 mm×100 mm)分离,以0.1%甲酸水溶液-乙腈梯度洗脱,采用电喷雾负离子源(ESI-),多反应监测(MRM)扫描方式监测,外标法定量测定。【结果】葡糖醛酸、酒石酸、苹果酸、2-羟基丁酸钠、二苯乙醇酸、羟基辛酸、N-乙酰神经氨酸等7种化合物在50.0~2 000.0μg·L^(-1)的浓度范围内呈线性关系(r>0.995);羟基乙酸、乳酸、柠檬酸、扁桃酸等4种化合物在100.0~5 000.0μg·L^(-1)的浓度范围内呈线性关系(r>0.995);乳糖酸、葡糖酸等2种化合物在50.0~5 000.0μg·L^(-1)的浓度范围内呈线性关系(r>0.995)。考察了水剂、膏霜、乳液类化妆品的加标回收率。回收率结果在92.3%~114.1%,相对标准偏差(RSD)在0.9%~6.0%。葡糖醛酸、酒石酸、苹果酸、柠檬酸、2-羟基丁酸、二苯乙醇酸、羟基辛酸、乳糖酸、葡糖酸、N-乙酰神经氨酸的方法检出限均为0.003%;羟基乙酸、乳酸、扁桃酸的方法检出限均为0.006%。10批市售化妆品中8批为阳性。【结论】UHPLC-MS/MS法高效、灵敏、准确,适用于化妆品中葡糖醛酸、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、乳糖酸、葡糖酸、N-乙酰神经氨酸等13种α-羟基酸的检测。[Objective]To establish a UHPLC-MS/MS quantitative method for the determination of glucuronic acid,tartaric acid,glycolic acid,malic acid,lactic acid,citric acid,DL-2-hydroxybutyric acid sodium,mandelic acid,benzilic acid,hydroxycaprylic acid,lactobionic acid,gluconic acid and N-acetylneuraminic acid in cosmetics.[Methods]Samples were prepared by ultrasonic extraction,cleansed by precipitating reagent and followed by high-speed centrifugation of the extraction solution.The supernatant was filtered by 0.22μm Millipore filter.The continued filtrate was taken for analysis.A reversed phase column,Poroshell 120 EC-C18(2.7μm,4.6 mm×1000 mm)was used with 0.1%formic acid buffer and acetonitrile as the mobile phase under the condition of gradient elution.The analytes were detected with electrospray ionization source in negative ion mode(ESI−)and multiple reactions monitoring(MRM),and quantified by external standard curve.[Results]The method showed a good linearity of glucuronic acid,tartaric acid,malic acid,DL-2-hydroxybutyric acid sodium,benzilic acid,hydroxycaprylic acid and N-acetylneuraminic acid within the concentration range of 50.0‒2000.0μg·L^(-1)(r>0.995).The method showed a good linearity of glycolic acid,lactic acid,citric acid and mandelic acid within the concentration range of 100.0‒5000.0μg·L^(-1)(r>0.995).The method showed a good linearity of lactobionic acid and gluconic acid within the concentration range of 50.0‒5000.0μg·L^(-1)(r>0.995).The recoveries were in the range of 92.3%‒114.1%;the relative standard deviations(RSD)were in the range of 0.9%‒6.0%(n=3).The detection limits of glucuronic acid,tartaric acid,malic acid,citric acid,DL-2-hydroxybutyric acid sodium,mandelic acid,benzilic acid,hydroxycaprylic acid,lactobionic acid,gluconic acid and N-acetylneuraminic acid were 0.003%while the detection limits of glycolic acid,lactic acid and mandelic acid were 0.006%.In 10 batches of commercially available cosmetics,eight batches showed positive result.[Conclusion]The UHPLC-MS/MS method

关 键 词：超高效液相色谱-串联质谱法 化妆品 Α-羟基酸 成分 

分 类 号：R115[医药卫生—公共卫生与预防医学]