Vosough Maryam, Shekari Nafiseh, Salemi Amir, Heidar Koorosh Tabar
Chemistry and Chemical Engineering Research Center of Iran, PO Box 14335-186, Tehran, Iran.
Shahid Beheshti University, Environmental Sciences Research Institute, Department of Environmental Technologies, 19839-63113 Tehran, Iran.
J AOAC Int. 2017 Mar 1;100(2):377-386. doi: 10.5740/jaoacint.16-0209. Epub 2016 Nov 30.
In the present study, a fast LC method coupled with multivariate curve resolution (MCR) alternating least-squares (ALS) and alternating trilinear decomposition (ATLD) was developed for the determination of the resolution of and quantitation of benzophenone-3, 4-methylbenzylidene camphor, octocrylene, ethylhexyl dimethyl para-aminobenzoic acid, butyl methoxydibenzoilmethane, and methyl and propyl parabens in suncare products. Chromatographic separation was optimized using full factorial and Box-Behnken designs. MCR-ALS and ATLD performance in quantitating the analytes in synthetic mixtures (which were randomly prepared in ultra-pure water) and blank sunscreen products was studied, and satisfying results were obtained. Acceptable qualification and quantification results were also achieved in the presence of matrix interferences via a short chromatographic runtime (5 min), and the second-order advantage was fully exploited, with MCR-ALS clearly emerging as the superior model. Average recoveries ranged from 98.0 to 112.5%, and RSD values were lower than 6.5%. LODs between 0.066 and 0.243 μg/g were achieved. In addition to acceptable precision and accuracy, the merits of the proposed method are that the analysis is fast and there is minimal solvent consumption. Moreover, coelution of analytes and interference from components in the sample matrixes were overcome with multivariate analysis.
在本研究中，开发了一种快速液相色谱法，结合多元曲线分辨（MCR）交替最小二乘法（ALS）和交替三线性分解（ATLD），用于测定防晒产品中二苯甲酮-3、4-甲基亚苄基樟脑、二乙氨羟苯甲酰基苯甲酸己酯、乙基己基二甲基对氨基苯甲酸、丁基甲氧基二苯甲酰甲烷以及对羟基苯甲酸甲酯和丙酯的分离度和进行定量分析。使用全因子设计和Box-Behnken设计对色谱分离进行了优化。研究了MCR-ALS和ATLD在定量合成混合物（在超纯水中随机配制）和空白防晒产品中分析物时的性能，并获得了满意的结果。在存在基质干扰的情况下，通过短色谱运行时间（5分钟）也获得了可接受的定性和定量结果，并且充分利用了二阶优势，MCR-ALS明显成为更优的模型。平均回收率在98.0%至112.5%之间，相对标准偏差值低于6.5%。检测限在0.066至0.243μg/g之间。除了具有可接受的精密度和准确度外，该方法的优点还包括分析速度快且溶剂消耗最少。此外，通过多元分析克服了分析物的共洗脱和样品基质中成分的干扰。
