The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and1Hwith sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin.The derivative was extracted using pentane and analyzed by the LC/MS. For the 1H NMR analysis, samplewas directly dissolved in D2O solvent without pretreatment. The quantitative analysis of glycerin was doneby 1H NMR ERETIC method. The analysis results of LC/MS and 1H NMR showed that the calibrationcurves were a good linearity with r2 = 0.9991 in the range of 0.1 to 10 g/mL and r2 = 1 in the rangeof 25 to 500 g/mL, respectively.