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分散液液微萃取结合高效液相色谱法同时分析中药中苦参生物碱

Dispersive Liquid-Liquid Microextraction Combined with High-Performance Liquid Chromatography for the Simultaneous Analysis of Matrine Alkaloids in Traditional Chinese Medicine.

作者信息

Zhang Ruxin, Hu Shuang, Chen Xuan, Bai Xiaohong

出版信息

J Chromatogr Sci. 2016 Oct 17;54(9):1687-1693. doi: 10.1093/chromsci/bmw114.

Abstract

Dispersive liquid-liquid microextraction (DLLME), coupled with high-performance liquid chromatography (HPLC), was developed and introduced for simultaneous extraction and determination of the trace level matrine alkaloids (oxymatrine, matrine, sophoridine and oxysophocarpine) in Composite Kushen Injection and Sophorae Flavescentis Radix. Several factors affecting performance were investigated and optimized, including type and volume of extraction solvent, type and volume of disperser solvent, sample phase pH, shaking time, centrifugation time and rate, and salt concentration in the sample solution. Under optimized conditions, the enrichment factors of DLLME for four matrine alkaloids ranged from 0.17 to 83.5; the good linearities were obtained for all analytes with the coefficient of determination of between 0.9924 and 0.9989; the limits of detection were between 0.2 and 275 ng mL-1; the satisfactory recoveries (86.6-104.5%) and the precision (relative standard deviation (RSD) 2.0-12.2%) were also achieved. The average content of sophoridine, oxymatrine, matrine and oxysophocarpine in Composite Kushen Injection and Sophorae Flavescentis Radix are 0.60, 40.3, 0.17, 0.39 mg mL-1 with the RSD of 5.3-9.0% (n = 3), and 0.13, 26.7, 1.20, 0.40 mg g-1 with the RSD of 3.5-9.2% (n = 3). The experimental results showed that the method was a simple, sensitive and practical for simultaneous extracting, enriching and quantifying of the different concentrations level matrine alkaloids in TCM.

摘要

建立了分散液液微萃取(DLLME)结合高效液相色谱(HPLC)的方法,用于同时萃取和测定复方苦参注射液和苦参中痕量的苦参生物碱(氧化苦参碱、苦参碱、槐定碱和氧化槐果碱)。考察并优化了影响萃取性能的多个因素,包括萃取溶剂的类型和体积、分散剂溶剂的类型和体积、样品相pH值、振荡时间、离心时间和速率以及样品溶液中的盐浓度。在优化条件下,DLLME对四种苦参生物碱的富集因子在0.17至83.5之间;所有分析物均具有良好的线性关系,测定系数在0.9924至0.9989之间;检测限在0.2至275 ng mL-1之间;回收率也令人满意(86.6 - 104.5%),精密度(相对标准偏差(RSD)为2.0 - 12.2%)。复方苦参注射液和苦参中槐定碱、氧化苦参碱、苦参碱和氧化槐果碱的平均含量分别为0.60、40.3、0.17、0.39 mg mL-1,RSD为5.3 - 9.0%(n = 3),以及0.13、26.7、1.20、0.40 mg g-1,RSD为3.5 - 9.2%(n = 3)。实验结果表明,该方法简便、灵敏、实用,可用于同时萃取、富集和定量中药中不同浓度水平的苦参生物碱。

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