2次元NMRによる化粧品中の紫外線吸収剤の分析

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Simple and reliable methods for the qualitative and quantitative analysis of ultraviolet (UV) absorbers in cosmetics by two dimension NMR (2D-NMR) were presented. The procedure consists of the following direct method for the samples containing more than 2% of UV absorbers and of the concentration method for the samples containing less than 2% of UV absorbers. The direct method : One hundred to 300 mg of cosmetics was weighed, placed into a test tube, and added 2 ml of saturated sodium chloride solution and 1 ml of the CDCl_3 solution containing 1% of pyrazine and 0.5% of tetramethylsilane. The mixture was shaken for 10 min. and centrifuged at 3000 rpm for 10 min. The CDCl_3 solution was transferred into a NMR tube. The concentration method : Five to 50 g of samples was weighed, placed into a 200 ml separating funnel, added 80 ml of saturated sodium chloride solution, and extracted with 30 ml of chloroform for 3 times. The chloroform layer was evaporated to dryness under reduced pressure. The residue was dissolved in 1 ml of the CDCl_3 solution for NMR measurements as described in the direct method. The ^<13>C-^1H heteronuclear shift correlated NMR spectra (HETCOR) of UV absorbers in the CDCl_3 solution were measured for the simultaneous qualitative analysis of UV absorbers by the fingerprint identification, and the relative integral intensity in their ^1H-NMR signals was used for the quantitative analysis using pyrazine as an internal standard. The proposed methods were successfully applied to the analysis of UV absorbers in cosmetics.
社団法人日本薬学会の論文
1996-02-29

2次元NMRによる化粧品中の紫外線吸収剤の分析

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