超高效液相色谱-串联质谱法测定化妆品中乳糖酸等8种有机酸

Determination of eight organic acids such as lactobionic acid in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定化妆品中乳糖酸、L-乳酸、柠檬酸、丁二酸、DL-扁桃酸、阿魏酸、壬二酸和硫辛酸8种有机酸含量。以甲醇-水(体积比50∶50)为提取液,用UPLC-MS/MS进行分析,乙酸铵(pH值=2.6)-水-乙腈为流动相,梯度洗脱,流速为0.35 mL/min,柱温35℃,采用ACQUITY UPLC®HSS T3柱(1.8μm,2.1 mm×100 mm)分离,负离子多反应监测(MRM)模式进行含量测定。乳糖酸、L-乳酸、柠檬酸、丁二酸、DL-扁桃酸、阿魏酸、壬二酸和硫辛酸分别在2.52~10.10,4.54~18.16,2.82~15.30,2.30~9.22,2.41~9.63,2.27~9.08,2.33~9.33,2.16~8.65μg/mL范围内与峰面积线性关系良好(R2≥0.99);检出限达到0.003μg/g。精密度、稳定性、重复性试验的RSD均小于7.79%;高、中、低不同质量浓度的加标回收率在86.52%~119.98%之间,RSD在0.55%~4.74%之间。该方法准确度高、重复性好、速度快,适用于同时检测化妆品中乳糖酸等8种有机酸成分的含量。

The study aims to establish a method for the determination of eight organic acids in cosmetics,including lactobionic acid,L-lactic acid,citric acid,succinic acid,DL-mandelic acid,ferulic acid,azelaic acid and lipoic acid,by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The chromatographic column was Waters ACQUITY UPLC®HSS T3 column(1.8μm,2.1 mm×100 mm)with methanol-water(volume ratio 50∶50)as the extraction solution and ammonium acetate(pH=2.6)-water-acetonitrile as the mobile phases.The flow rate is 0.35 mL/min and the column temperature is 35℃.The electrospray ion(ESI)source,negative ions scanning method and multiple reaction monitoring(MRM)mode are used to determine the content.There are good linear relationships(R2≥0.99)and the peak area of the eight organic acids are 2.52-10.10,4.54-18.16,2.82-15.30,2.30-9.22,2.41-9.63,2.27-9.08,2.33-9.33,and 2.16-8.65μg/mL,respectively.Their minimum limits of quantitation(LOQ)are as low as 0.003μg/g.The RSDs of precision,stability and repeatability tests are all less than 7.79%.The recoveries of high,medium and low concentrations range from 86.52%to 119.98%,with RSD ranging from 0.55%to 4.74%.The method has high accuracy,good repeatability and fast speed,and is suitable for the simultaneous determination of eight organic acids in cosmetics.