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(1.8 μm, 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2.52~10.10,4.54~18.16,2.82~15.30,2.30~9.22,2.41~9.63,2.27~9.08,2.33~9.33,2.16~8.65 μg/mL范围内与峰面积线性关系良好(R2≥0.99);检出限达到0.003 μg/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 (1.8 μm, 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 2.16-8.65 μg/mL, respectively. Their minimum limits of quantitation (LOQ) are as low as 0.003 μg/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.