Xiong Chensihui, Ding Tianming, Liu Jie, Yi Ou, Ding Xiaoping, Xie Yun
School of Pharmaceutical Science, Hubei University of Chinese Medicine, Wuhan 430065, China.
Hubei Institute for Drug Control, Wuhan 430075, China.
Se Pu. 2022 Sep;40(9):817-824. doi: 10.3724/SP.J.1123.2022.03037.
Plant components from extracts of , rhodiola, ginseng, , and tea play important roles in skin whitening, moisturizing, anti-aging, sun protection, anti-inflammation, antiseptic, bacteriostatic, and other effects of cosmetics. At present, no relevant standard methods have been established to detect the addition amounts of plant extracts in cosmetics. In addition, plant extracts listed in product labels may be undetectable due to their addition in trace quantities and the lack of technical support. Therefore, a quantitative method for the simultaneous determination of 22 functional components in cosmetics was established by ultra-high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UHPLC-LTQ/Orbitrap MS). Target compounds were extracted with methanol from samples using ultrasonic extraction, and then separated on a C18 column (100 mm × 2.1 mm, 1.8 μm) with gradient elution of 0.1% (v/v) formic acid aqueous solution (A) and acetonitrile (B). The gradient elution program were as follows: 0-5 min, 5%B-8%B; 5-25 min, 8%B-60%B; 25-35 min, 60%B-80%B; 35-36 min, 80%B-5%B; 36-45 min, 5%B. The flow rate was 0.3 mL/min and the injection volume was 5 μL. Accurate masses of precursor ions were used to detect cosmetic functional components in positive ionization mode. The fragment ions obtained by higher energy collisional dissociation were used for confirmation of the functional components. Each compound showed good linearity. The limits of detection (LODs) were in the range of 0.003-2.01 mg/kg, and the limits of quantification (LOQs) were in the range of 0.02-4.36 mg/kg. Recoveries at three levels were 63.2%-125.1%, and relative standard deviations (RSDs) were 0.18%-10.9%. Fifty-four batches of samples labeled with four monomer functional components and nine plant extracts were tested. In the 17 batches of samples labeled with nicotinamide, 4 batches labeled with caffeine, and 6 batches labeled with root extract, the labeled functional components were detected. One out of 11 batches of samples labeled with D-panthenol was not detected. Three of the seven batches of samples labeled with ascorbyl glucoside were not detected. In the 21 batches of samples labeled with licorice extracts, the corresponding functional components were not detected in 9 batches. In the 21 batches of samples labeled with extract, the corresponding functional components were not detected in 11 batches. In the 13 batches of samples labeled with tea extract, the corresponding functional components were not detected in 8 batches. In 11 of the 12 batches containing ginseng root extract, the corresponding functional components were not detected. In five of the six batches of astragalus membranaceus root extract samples, the corresponding functional components were not detected. In samples labeled with root extract, root extract, and root extract, the corresponding functional components were detected. The method is simple, rapid, reliable, accurate, and suitable for the determination of the 22 functional components in cosmetics.
红景天、人参、[此处原文缺失植物名称]和茶叶提取物中的植物成分在化妆品的美白、保湿、抗老化、防晒、抗炎、防腐、抑菌等功效中发挥着重要作用。目前,尚未建立检测化妆品中植物提取物添加量的相关标准方法。此外,产品标签中列出的植物提取物可能因添加量极少且缺乏技术支持而无法检测到。因此,建立了一种超高效液相色谱 - 线性离子阱/轨道阱高分辨率质谱法(UHPLC - LTQ/Orbitrap MS)同时测定化妆品中22种功能成分的定量方法。目标化合物采用甲醇通过超声提取从样品中提取出来,然后在C18柱(100 mm×2.1 mm,1.8μm)上进行分离,以0.1%(v/v)甲酸水溶液(A)和乙腈(B)进行梯度洗脱。梯度洗脱程序如下:0 - 5分钟,5%B - 8%B;5 - 25分钟,8%B - 60%B;25 - 35分钟,60%B - 80%B;35 - 36分钟,80%B - 5%B;36 - 45分钟,5%B。流速为0.3 mL/min,进样量为5μL。在正离子模式下使用前体离子的精确质量数来检测化妆品功能成分。通过高能碰撞解离获得的碎片离子用于确认功能成分。每种化合物均表现出良好的线性关系。检测限(LOD)在0.003 - 2.01 mg/kg范围内,定量限(LOQ)在0.02 - 4.36 mg/kg范围内。三个加标水平的回收率为63.2% - 125.1%,相对标准偏差(RSD)为0.18% - 10.9%。对54批次标注有四种单体功能成分和九种植物提取物的样品进行了检测。在17批次标注烟酰胺的样品中,检测到了标注的功能成分;在4批次标注咖啡因的样品中,检测到了标注的功能成分;在6批次标注[此处原文缺失植物名称]根提取物的样品中,检测到了标注的功能成分。在11批次标注D - 泛醇的样品中,有1批次未检测到标注的功能成分。在7批次标注抗坏血酸葡糖苷的样品中,有3批次未检测到标注的功能成分。在21批次标注甘草提取物的样品中,有9批次未检测到相应的功能成分。在21批次标注[此处原文缺失植物名称]提取物的样品中,有11批次未检测到相应的功能成分。在13批次标注茶叶提取物的样品中,有8批次未检测到相应的功能成分。在12批次含人参根提取物的样品中,有11批次未检测到相应的功能成分。在6批次黄芪根提取物样品中,有5批次未检测到相应的功能成分。在标注[此处原文缺失植物名称]根提取物、[此处原文缺失植物名称]根提取物和[此处原文缺失植物名称]根提取物的样品中,检测到了相应的功能成分。该方法简便、快速、可靠、准确,适用于化妆品中22种功能成分的测定。