Department of Analytical Chemistry, Faculty of Pharmacy, Anadolu University, 26470, Eskisehir, Turkey.
Doping and Narcotic Compounds Analysis Laboratory, Faculty of Pharmacy, Anadolu University, 26470, Eskisehir, Turkey.
Comb Chem High Throughput Screen. 2021;24(3):352-365. doi: 10.2174/1386207323999200728121657.
The alkyl esters of p-hydroxybenzoic acid at the C-4 position, "the parabens," including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure.
On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methylparaben, ethylparaben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products.
The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%.
The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six samples and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples was 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.
对羟基苯甲酸的 C-4 位烷基酯，即“对羟基苯甲酸酯”，包括甲酯、乙酯、丙酯和丁酯，被广泛用作食品、化妆品和药品中的抗菌防腐剂。官方对这些化合物的使用规定使得对其进行分析对于评估其暴露量至关重要。
在此基础上，开展了本研究，以开发一种简单、选择性和廉价的高效液相色谱法，用于定量测定药品和化妆品中甲基对羟基苯甲酸酯、乙基对羟基苯甲酸酯（EP）、正丙基对羟基苯甲酸酯（NPP）、异丙基对羟基苯甲酸酯（IPP）、正丁基对羟基苯甲酸酯（NBP）、异丁基对羟基苯甲酸酯（IBP）和对羟基苯甲酸苄酯（BP）。
在使用 Phenomenex 公司的 C18 键合核壳硅胶颗粒柱（粒径 2.6 μm，150×3.0 mm）在流速梯度洗脱条件下实现了分析物的色谱分离。将样品作为 1.0 μL 的等分试样注入系统，并用光电二极管阵列检测器在 254nm 波长下检测化合物。使用该技术，可以在 250-2000ng/mL 的浓度范围内测定七种对羟基苯甲酸酯衍生物。该方法的回收率在 99.95-13.84%范围内，RSD 最大值为 3.95%。
该方法已得到充分验证，并成功应用于不同的药品和化妆品样品（n=16），包括糖浆、混悬剂、口腔喷雾剂、凝胶等。在六个样品中检测到至少一种对羟基苯甲酸酯衍生物，并进行了定量测定。在分析样品中发现的对羟基苯甲酸酯衍生物的最大含量为 321.7ng/mL，为 MP。据我们所知，这是第一个适用于药品和化妆品样品的 LC 方法。
