高效液相色谱法和质谱法检测和鉴定化妆品中5种羟基酸  

Determination of Five Hydroxy Acids in Cosmetics by High Performance Liquid Chromatography and Identification by Mass Spectrometry

作　　者：张雷 胡积东 王海瑞 孙乐 ZHANG Lei;HU Jidong;WANG Hairui;SUN Le(Suzhou Huabo Biological Testing Co.Ltd.,Suzhou 215000)

机构地区：[1]苏州华搏生物检测有限公司,江苏苏州215000

出　　处：《分析科学学报》2024年第3期364-368,共5页Journal of Analytical Science

摘　　要：建立了同时测定化妆品中乳糖酸、葡萄糖酸、甘油酸、丙酮酸、羟基丙二酸5种羟基酸含量的高效液相色谱法,并采用液相色谱-串联质谱法进行了鉴定。样品先用少量异丙醇分散,再经一级水提取后,以30 mmol/L乙酸铵水溶液(磷酸调节pH至2.9)-甲醇作为流动相,经ZORBAX SB-Aq(250 mm×4.6 mm×5μm)色谱柱分离,用二极管阵列检测器进行检测;若出现疑似阳性样品,则进一步采用液相色谱-串联质谱法进行确证,采用ESI离子源,在SRM负离子监测模式下分别确立了5种羟基酸组分的定量、定性离子以及离子对的相对丰度比。结果表明,5种羟基酸在各自浓度范围内线性关系良好,相关系数均大于0.999,检出浓度为30~100 mg/kg,定量浓度为120~300 mg/kg,平均加标回收率为91.8%~104.1%,RSD为0.1%~1.9%。该方法高效、准确、可靠,适用于化妆品中5种羟基酸组分的定性筛查及含量测定。An HPLC method and a LC-MS/MS method for the simultaneous determination of five hydroxy acid(lactobionic acid,gluconic acid,glyceric acid,pyruvic acid and hydroxymalonic acid)in cosmetics have been estabished.The sample was firstly dispersed with a small amount of isopropanol,and then extracted with primary water.A 30 mmol/L aqueous solution of ammonium acetate(adjusted to pH 2.9 with phosphoric acid)-methanol was used as the mobile phase,and the sample was subjected to ZORBAX SB-Aq(250 mm×4.6 mm×5μm)chromatographic column separation and detection using diode array detector;if there is a suspected positive sample,it should be further confirmed by liquid chromatography-tandem mass spectrometry,and the ESI ion source should be used to establish the quantitative and qualitative ions and the relative abundance ratio of ion pairs of the five hydroxy acid components under the SRM negative ion monitoring mode.The results showed that the linear relationship of the five hydroxy acids was good within their respective concentration ranges,the correlation coefficients were all greater than 0.999,the detection concentration was 30-100 mg/kg,the quantitative concentration was 120-300 mg/kg,the average standard addition recovery was 91.8%-104.1%,and the RSD was 0.1%-1.9%.The method is efficient,accurate and reliable.It is suitable for qualitative screening and content determination of five hydroxy acids in cosmetics.

关 键 词：羟基酸 高效液相色谱 高效液相色谱-串联质谱 化妆品 

分 类 号：O657.63[理学—分析化学]