建立并验证了一种反相高效液相色谱法，用于定量和稳定检测化妆品乳膏中的α-硫辛酸。
Development and validation of a reversed-phase high-performance liquid chromatographic method for the quantitation and stability of α-lipoic acid in cosmetic creams.
机构信息
Department of Biomedical Sciences, Faculty of Health and Welfare Sciences, Division of Aesthetics and Cosmetic Science, University of West Attica, Campus 1, Agiou Spyridonos, Egaleo, Athens, 12243, Greece.
Laboratory of Pharmaceutical Analysis, Division of Pharmaceutical Chemistry, Faculty of Pharmacy, National and Kapodistrian University of Athens, Panepistimipolis - Zografou, Athens, 15771, Greece.
出版信息
Int J Cosmet Sci. 2020 Jun;42(3):221-228. doi: 10.1111/ics.12603. Epub 2020 Apr 13.
OBJECTIVE
To develop and validate a simple reversed-phase HPLC method for the quantitation and evaluation of stability of α-lipoic acid in cosmetics, according to International Conference on Harmonization (ICH) Guidelines.
METHODS
The chromatography was performed on a reversed-phase Luna C18, analytical column (150 × 4.6 mm id, 5 μm particle size) with a mobile phase of potassium dihydrogen phosphate (pΗ 4.5; 0.05 M) and acetonitrile (60:40, v/v) and a flow rate of 1.0 mL min with UV detection at 340 nm. Accelerated and long-term stability studies of α-lipoic acid in cosmetic cream were conducted under various degradation conditions including acid, basis, oxidation, and thermal and photolytic degradation, according to European Medicines Agency Guidelines CPMP/ICH/2736/99.
RESULTS
The limit of detection (LOD) for the cosmetic cream was 0.9 μg mL and the limit of quantitation (LOQ) was 2.8 μg mL , while the retention time was 7.2 min. The method proved to be linear, precise and accurate. The stability results demonstrated the selectivity of the proposed method to the analysis of α-LA, and the degradation products were determined and evaluated in specific stress conditions in cosmetic creams. The applicability of the method was tested in two different developed cosmetic products (cream with 1.5 % w/w and emulsion with 1.0 % w/w of LA) and proved to be reliable.
CONCLUSION
A reversed-phase HPLC-UV method was developed and fully validated for the analysis of α-lipoic acid in cosmetics. It is the first reported application on the quantitation of lipoic acid in cosmetic creams, while at the same time evaluates the stability in forced degradation conditions, in new cosmetic formulations. It proved to be suitable for the reliable quality control of cosmetic products, with a run time of <8 min that allows for the analysis of large number of samples per day.
目的
根据国际人用药品注册技术协调会（ICH）指导原则，开发并验证一种用于化妆品中α-硫辛酸定量分析和稳定性评估的反相高效液相色谱（HPLC）方法。
方法
采用反相 Luna C18 分析柱（150×4.6mm id，5μm 粒径），以磷酸二氢钾（pH 4.5；0.05M）-乙腈（60:40，v/v）为流动相，流速为 1.0mL/min，在 340nm 处进行紫外检测，对化妆品乳膏中α-硫辛酸进行加速和长期稳定性研究。根据欧洲药品管理局（EMA）CPMP/ICH/2736/99 指导原则，在各种降解条件下（包括酸、碱、氧化、热和光降解）进行稳定性研究。
结果
该方法在化妆品乳膏中的检测限（LOD）为 0.9μg/mL，定量限（LOQ）为 2.8μg/mL，保留时间为 7.2min。方法证明具有良好的线性、精密度和准确性。稳定性研究结果表明，该方法对α-LA 分析具有选择性，在化妆品乳膏的特定条件下确定并评估了降解产物。该方法的适用性在两种不同开发的化妆品产品（含 1.5%w/w 的乳膏和含 1.0%w/w 的乳剂）中进行了测试，结果可靠。
结论
建立了一种反相 HPLC-UV 方法，用于化妆品中α-硫辛酸的分析。这是首次报道用于化妆品乳膏中硫辛酸定量分析的方法，同时在新的化妆品配方中，评估了强制降解条件下的稳定性。该方法证明适用于化妆品产品的可靠质量控制，运行时间<8min，每天可分析大量样品。
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