School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
J Chromatogr A. 2018 Jun 15;1554:37-44. doi: 10.1016/j.chroma.2018.04.021. Epub 2018 Apr 18.
Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics.
如今，化妆品的安全性是一个广泛关注的问题。胺类是常见的化妆品添加剂。其中一些，如氨基酸，是有益的。然而，另一种胺类，ε-氨基己酸（EACA）因其不良反应而被禁止添加到化妆品中。在这项研究中，开发了一种简单、快速、灵敏和环保的一步超声辅助提取和衍生化（UAE-D）方法，用于通过高效液相色谱（HPLC）结合测定化妆品中的 EACA 和氨基酸。通过使用这种样品制备方法，EACA 和氨基酸的提取和衍生化在超声场中一步完成。在这个过程中，4-氟-7-硝基苯并呋咱（NBD-F）被用作衍生化试剂。评估了提取条件，包括 NBD-F 的用量、提取和衍生化温度、超声振动时间和水相的 pH 值。同时，还研究了提取机制。在优化条件下，该方法的检测限为 0.086-0.15μg/L，定量限为 0.29-0.47μg/L，相对标准偏差（RSD）小于 3.7%（n=3）。从化妆品样品中获得的 EACA 和氨基酸回收率在 76.9%-122.3%之间。在所有选定的样品中都发现了氨基酸，并定量在 1.9±0.9 到 677.2±17.9μg/kg 之间。在一个粉饼样品中发现并定量了 EACA，其含量为 1284.3±22.1μg/kg。这种 UAE-D-HPLC 方法缩短并简化了样品预处理，并提高了分析方法的灵敏度。在我们的记录中，总样品制备过程仅需 10 分钟。并且方法检测限比文献报道低两个数量级。此外，我们减少了溶剂的消耗并尽量减少有机溶剂的使用，使我们的方法朝着绿色分析化学的方向发展。总之，我们的 UAE-D-HPLC 方法是一种简单、快速、灵敏和环保的分析方法，用于测定化妆品中的 EACA 和氨基酸。
