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采用定量 1H NMR 法直接测定柴胡中柴胡皂苷的含量。

Quantitative H NMR for the Direct Quantification of Saikosaponins in Bupleurum chinense DC.

机构信息

School of Pharmacy and Chemical Engineering, Zhengzhou University of Industrial Technology, Zhengzhou, 451100, China.

High & New Technology Research Center of Henan Academy of Sciences, Zhengzhou, 450002, China.

出版信息

Anal Sci. 2021 Oct 10;37(10):1413-1418. doi: 10.2116/analsci.20P462. Epub 2021 Mar 26.

Abstract

Saikosaponin a and saikosaponin d are used as chemical standards for the quality evaluation of Bupleurum chinense DC. by the high-performance liquid chromatography method in current Chinese Pharmacopoeia. However, other saikosaponins, such as saikosaponin c and saikosaponin b, also possess pharmaceutical activity, but are not used as chemical standards. In this study, a quantitative proton nuclear magnetic resonance (H NMR) method was developed to determine the total mass percentage (mg/g) of SSa, SSb, SSb and SSd in B. chinense DC., using the H-24 (δ 0.71) signal. Furthermore, the molality (mol/kg) of type I saikosaponins (epoxy-ether structure) was also determined by quantitative H NMR in the area of H-11 (δ 5.95) for a more accurate quality evaluation. Validation of the method confirmed that it has acceptable selectivity, precision, stability, and repeatability. The results indicated that this method has the potential to be a reliable method for the quantification of saikosaponins in Bupleurum scorzonerifolium Willd., vinegar baked B. chinense DC. and B. scorzonerifolium Willd., Chaihu Koufuye (oral liquid of Chaihu).

摘要

柴胡属中柴苷 A 和柴苷 D 被用作《中国药典》中质量评价的化学标准。然而,其他柴胡皂苷,如柴胡皂苷 C 和柴胡皂苷 B,也具有药用活性,但不作为化学标准使用。本研究建立了一种定量质子核磁共振(1H NMR)法,以 0.71 的 H-24 信号为内标,测定柴胡中 SSa、SSb、SSb 和 SSd 的总质量百分比(mg/g)。此外,还通过 1H NMR 在 H-11(δ 5.95)区域测定了 I 型柴胡皂苷(环氧化醚结构)的克分子浓度(mol/kg),以进行更准确的质量评价。方法验证表明,该方法具有良好的选择性、精密度、稳定性和重现性。结果表明,该方法有望成为定量测定醋制柴胡、醋炙柴胡和柴黄口服液中柴胡皂苷的可靠方法。

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