Whitening is a core function of cosmetics, and ingredients including acetyl glucosamine, tranexamic acid, nicotinamide, phenethyl resorcinol, glabridin, and ascorbyl tetraisopalmitate are widely used due to their clearly established whitening mechanisms. However, existing analytical methods face notable limitations: photodiode array detectors (PDA) cannot reliably detect weakly or non-ultraviolet (UV)-absorbing components; evaporative light scattering detectors (ELSD) suffer from inadequate sensitivity for low-concentration analytes; mass spectrometry (MS) is costly; and single-column cannot achieve the separation of ingredients with significantly different polarities. To address these challenges, this study established an analytical method for the determination of the six whitening ingredients in cosmetics using ultra performance liquid chromatography coupled with a photodiode array detector and a corona charged aerosol detector (UPLC-PDA-CAD). For sample pretreatment: 0.2 g of sample was weighed, and 10 mL dichloromethane and 10 mL deionized water were added for vortex extraction of whitening ingredients. The mixture was then centrifuged for phase separation. The aqueous layer and dichloromethane layer were collected separately. The aqueous layer was washed twice with dichloromethane; all dichloromethane fractions were combined, concentrated to less than 1 mL under a nitrogen stream, and finally made up to volume with isopropanol. Both the aqueous layer and the reconstituted isopropanol solution were filtered through 0.22 μm hydrophilic polytetrafluoroethylene (PTFE) membranes before UPLC injection. For chromatographic separation, a Waters HSS T3 column (150 mm×2.1 mm, 1.7 μm) was selected. The column temperature was set at 40 ℃, the injection volume was 1 μL, and the flow rate was 0.3 mL/min. The mobile phase consisted of isopropanol, acetonitrile, and 20 mmol/L ammonium acetate solution (pH adjusted to 4.5 using formic acid), using a gradient elution program. For detection, a tandem PDA-CAD system was used: PDA (scan range 200-400 nm) was employed for components with UV absorption, while CAD (nebulization temperature 35 °C, acquisition frequency 5 Hz) was used for components with weak UV absorption. Quantification was performed using the external standard method.Method validation results showed good linear relationships for all six whitening ingredients within their respective concentration ranges. The correlation coefficients (r) were all greater than 0.999. The limits of detection (LODs, S/N=3) were 5.0-50.0 µg/g, and the limits of quantification (LOQs, S/N=10) were 12.0-120.0 µg/g. Spiked recovery tests were conducted on negative cosmetic matrices (emulsion, cream, oil) at low, medium, and high levels. The recoveries ranged from 92.8% to 110.1%, and the relative standard deviations (RSDs, n=6) were 0.12%-5.45%, indicating excellent precision and accuracy. This method was applied to seven commercially cosmetics. The results revealed that all target whitening ingredients declared on the product labels were detected, with significant differences in their content. Nicotinamide was the most frequently detected compound, found in five products, and also exhibited the highest concentrations, ranging from 0.19% to 2.29%. Phenethyl resorcinol was detected in three products, with contents ranging from 0.02% to 0.52%. Ascorbyl tetraisopalmitate was detected in two products, at 0.09% and 3.08%, respectively. Acetyl glucosamine, tranexamic acid, and glabridin were each detected in only one product. In conclusion, this established UPLC-PDA-CAD method is simple, efficient, sensitive and accurate. It effectively overcomes the technical challenge of detecting whitening ingredients with widely varying polarities, offering reliable technical support for cosmetic quality control, regulatory supervision, and evaluation of product whitening efficacy and potential sensitization risks. 建立了一种超高效液相色谱-二极管阵列检测器串联电雾式检测器(UPLC-PDA-CAD)测定化妆品中乙酰壳糖胺、氨甲环酸、烟酰胺、苯乙基间苯二酚、光甘草定及抗坏血酸四异棕榈酸酯6种美白成分的分析方法。样品用二氯甲烷和水涡旋提取,收集二氯甲烷层和水层;水层经二氯甲烷洗涤后,合并二氯甲烷相,氮吹浓缩至<1 mL并以异丙醇定容。水层和异丙醇定容液分别过滤,注入液相色谱仪,通过Waters HSS T3柱(150 mm×2.1 mm,1.7 μm)分离。流动相为异丙醇-乙腈-20 mmol/L乙酸铵缓冲液(甲酸调节pH至4.0),采用梯度洗脱方式,以二极管阵列检测器串联电雾式检测器进行检测,外标法定量。分别对样品前处理方法和色谱条件进行了优化。在优化的实验条件下,6种美白功效成分在一定范围内线性关系良好,相关系数(r)均>0.999,在乳、霜、油3种化妆品基质中的加标回收率为92.8%~110.1%,相对标准偏差(RSD,n=6)为0.12%~5.54%。对市售的7款化妆品进行检测,检出的美白成分与产品包装标示成分一致,但各成分含量差异较大。烟酰胺的使用频率和测得含量均较高,5款产品的测试结果为0.19%~2.29%。该方法操作简便,稳定可靠,重复性好,适用于化妆品中这几种极性差异显著的美白成分的检测。
使用 AI 将内容摘要翻译为中文,便于快速阅读
使用 AI 分析这篇文章的核心发现、关键要点和深度见解
由 DeepSeek AI 提供分析 · 首次使用需配置 API Key
arXiv · 2025-01-14
arXiv · 2026-01-28