Guohua Xia, Pan Ruirong, Bao Rui, Ge Yanru, Zhou Cunshan, Shen Yuping
Department of Food Sciences, School of Food Sciences and Engineering, Jiangsu University, Zhenjiang, Jiangsu, P.R. China.
Department of Chinese Materia Medica and Pharmacy, School of Pharmacy, Jiangsu University, Zhenjiang, Jiangsu, P.R. China.
Pharmacogn Mag. 2017 Oct-Dec;13(52):659-662. doi: 10.4103/pm.pm_350_16. Epub 2017 Nov 13.
Sanghuang is one of mystical traditional Chinese medicines recorded earliest 2000 years ago, that included various fungi of genus and was well-known for antitumor effect in modern medicine. is grown in natural forest of Northeastern China merely and used as Sanghuang commercially, but it has no quality control specification until now. This study was to establish a rapid method of two-phase acid hydrolysis followed by reversed phase-high performance liquid chromatography-ultra violet (RP-HPLC-UV) to quantify naringenin in the fruit body of .
Sample solution was prepared by pretreatment of raw material in two-phase acid hydrolysis and the hydrolysis technology was optimized. After reconstitution, analysis was performed using RP-HPLC-UV. The method validation was investigated and the naringenin content of sample and comparison were determined.
The naringenin was obtained by two-phase acid hydrolysis method, namely, 10.0 g of raw material was hydrolyzed in 200 mL of 1% sulfuric acid aqueous solution (v/v) and 400 mL of chloroform in oil bath at 110°C for 2 h. Good linearity ( = 0.9992) was achieved between concentration of analyte and peak area. The relative standard deviation (RSD) of precision was 2.47% and the RSD of naringenin contents for repeatability was 3.13%. The accuracy was supported with recoveries at 96.37%, 97.30%, and 99.31%. The sample solution prepared using the proposed method contained higher content of naringenin than conventional method and was stable for 8 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 naringenin in the fungus.
A convenient two-phase acid hydrolysis was employed to produce naringenin from raw material, and then an efficient and reliable reversed phase-high performance liquid chromatography-ultra violet method was established to monitor naringenin in the fruit bodies of . The newly established method could be used to control the quality of the herb. RP-HPLC-UV: Reversed Phase-High Performance Liquid Chromatography-Ultra Violet, RSD: Relative Standard Deviation, EtOAc: Ethyl acetate, ACN: Acetonitrile, MeOH: Methanol, RH: Relative Humility.
桑黄是2000年前最早记载的神秘传统中药之一，它包含多种属的真菌，在现代医学中以抗肿瘤作用而闻名。它仅生长在中国东北的天然森林中，并作为桑黄进行商业使用，但至今尚无质量控制规范。本研究旨在建立一种快速的两相酸水解后反相高效液相色谱-紫外检测法（RP-HPLC-UV）来定量桑黄子实体中的柚皮素。
通过对原料进行两相酸水解预处理制备样品溶液，并对水解工艺进行优化。复溶后，采用RP-HPLC-UV进行分析。考察方法的验证情况，并测定样品和对照品中柚皮素的含量。
采用两相酸水解法得到柚皮素，即10.0 g原料在200 mL 1%硫酸水溶液（v/v）和400 mL氯仿中于110°C油浴水解2 h。分析物浓度与峰面积之间具有良好的线性关系（r = 0.9992）。精密度的相对标准偏差（RSD）为2.47%，柚皮素含量重复性的RSD为3.13%。回收率分别为96.37%、97.30%和99.31%，证明了方法的准确性。所建立方法制备的样品溶液中柚皮素含量高于传统方法，且在8 h内稳定。
由于样品前处理效率高且HPLC方法可靠性高，该方法用于该真菌中柚皮素的常规分析是可行的。
采用简便的两相酸水解从原料中制备柚皮素，然后建立了高效可靠的反相高效液相色谱-紫外检测法来监测桑黄子实体中的柚皮素。新建立的方法可用于控制该药材的质量。RP-HPLC-UV：反相高效液相色谱-紫外检测，RSD：相对标准偏差，EtOAc：乙酸乙酯，ACN：乙腈，MeOH：甲醇，RH：相对湿度。
