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采用纤维素酶解与两相酸水解串联耦合技术,结合高效液相色谱-紫外检测法快速定量分析盾叶薯蓣块茎中的薯蓣皂苷元。

Rapid quantitative analysis of diosgenin in the tubers of Dioscorea zingiberensis C.H. Wright by coupling cellulose enzymolysis and two-phase acid hydrolysis in tandem with HPLC-UV.

机构信息

a School of Pharmacy, Jiangsu University , Zhenjiang , 212013 , P.R. China.

出版信息

Nat Prod Res. 2013 Oct;27(20):1933-5. doi: 10.1080/14786419.2013.790030. Epub 2013 May 14.

Abstract

A rapid method was developed to quantify diosgenin in Rhizoma Dioscoreae Zingiberensis. For the first time, sample solution was prepared by coupling pretreatment of raw material in cellulase and two-phase acid hydrolysis. After reconstitution, analysis was carried out on a C18 column, at 30°C, with acetonitrile and water (70:30, v/v) as mobile phase with flow rate of 1.0 mL min(- 1). Detection was carried out at 202 nm. Good linearity (r(2) = 0.9998) was established between concentration of analyte and peak area. The precision was >99% and the RSD of diosgenin contents for repeatability was 1.81%. The accuracy was supported with recoveries at 98.8%, 101.6% and 101.2%. The sample solution prepared using the proposed method contained higher content of diosgenin and was stable for 48 h. Due to the high efficiency of sample preparation and high reliability of the HPLC method, it is feasible to use this method for routine analysis of diosgenin in the herb.

摘要

建立了一种快速测定盾叶薯蓣中薯蓣皂苷元的方法。首次采用纤维素酶结合两相酸水解对原料进行预处理来制备供试品溶液。在 30℃下,以乙腈-水(70:30,v/v)为流动相,流速为 1.0ml/min,在 C18 柱上进行分析。检测波长为 202nm。分析物浓度与峰面积之间呈良好的线性关系(r²=0.9998)。精密度>99%,重复性测定的薯蓣皂苷元含量的 RSD 为 1.81%。该方法的准确度用 98.8%、101.6%和 101.2%的回收率得到支持。与传统方法相比,所建立的方法具有样品处理效率高、分析结果准确可靠等优点,可用于盾叶薯蓣中薯蓣皂苷元的常规分析。

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