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. 2013 Dec;3(6):456-459.
doi: 10.1016/j.jpha.2013.07.004. Epub 2013 Aug 7.

Preparative isolation of Heteroclitin D from Kadsurae Caulis using normal-phase flash chromatography

Xiao-Xue Yu  1   2 , Qian-Wen Wang  1 , Xin-Jun Xu  1   2 , Wei-Jian Lv  1   2 , Ming-Qian Zhao  1   2 , Zhi-Kun Liang  1   2
Affiliations

Preparative isolation of Heteroclitin D from Kadsurae Caulis using normal-phase flash chromatography

Xiao-Xue Yu et al. J Pharm Anal. 2013 Dec.

Abstract

Heteroclitin D (H.D) was successfully isolated from Kadsurae Caulis by using flash chromatography and recrystallized by methanol, 10.2 mg of H.D was obtained from 4.86 g of crude extract, and the purity determined by HPLC was 99.4%. The structure was identified by UV, IR, MS, and NMR analysis. The fast, simple and efficient method can be applied to the preparation of reference substance of H. D.

Keywords: Heteroclitin D; Kadsurae Caulis; Normal-phase flash chromatography.

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Figures

Fig. 1
Fig. 1
Flash chromatogram of Kadsurae Caulis extract (Peak 3 was Heteroclitin D determined by HPLC).
Fig. 2
Fig. 2
HPLC chromatogram of Heteroclitin D (purity 99.4%).
Fig. 3
Fig. 3
Comparison among flash chromatography methods ((A) 35% ethyl acetate, (B) 38% ethyl acetate and (C) 40% ethyl acetate).
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