1 Results Layered Double Hydroxide (LDH) finds extensive usage in the areas of pharmaceutical sciences and catalysis. In this study, a member of the LDH family, Mg/Al-hydrotalcite (HT), or the so-called anionic clay, was prepared at ratio 4 (HT) by co-precipitating through continuous agitation. X-ray diffraction pattern and thermogravimetric analysis of the material indicated that a pure HT had been successfully synthesized. This matrix was then used as support in the immobilization of lipase from Candida rugosa. Immobilization onto this matrix showed successful enhancement of lipase enantioselectivity. High yield (54.35%) and optical purity (81.51%) was achieved at 30 ℃, after 24 hours of reaction in hexane. Resolution of (±)-menthol depended on the moderate water activity (0.53) and operational stability of the LDH-lipase (Candida rugosa lipase immobilized onto HT) in catalysis of the esterification reaction showed > 60% recovery after 12 days of repeated use. The resolution of racemic menthol by the LDH-lipase catalyzed esterification is very convenient, representing a significant improvement in the use of enzyme for the preparative production of optically active menthol. 1 Results Layered Double Hydroxide (LDH) has found extensive usage in the areas of pharmaceutical sciences and catalysis. In this study, a member of the LDH family, Mg / Al-hydrotalcite (HT), or the so-called anionic clay, was prepared at ratio 4 (HT) by co-precipitating through continuous agitation. X-ray diffraction pattern and thermogravimetric analysis of the material indicated that a pure HT had been synthesized. This matrix was then used as support in the immobilization of lipase from Candida rugosa High yield (54.35%) and optical purity (81.51%) was achieved at 30 ° C after 24 hours of reaction in hexane. Resolution of (±) -menthol depended on the moderate water activity (0.53) and operational stability of the LDH-lipase (Candida rugosa lipase immobilized onto HT) in catalysis of the esterification reaction showed> 60% recovery after 12 days of repeated use. The resolution of racemic menthol by the LDH-lipase catalyzed esterification is very convenient, representing a significant improvement in the use of enzyme for the preparative production of optically active menthol.