Exploration of a ternary deep eutectic solvent of methyltriphenylphosphonium bromide/chalcone/formic acid for the selective recognition of rutin and quercetin in Herba Artemisiae Scopariae

Methyltriphenylphosphonium bromide/chalcone/formic acid, a green ternary deep eutectic solvent, was applied as a functional monomer and dummy template simultaneously in the synthesis of a new molecularly imprinted polymer. Ternary deep eutectic solvent based molecularly imprinted polymers are used as a solid‐phase extraction sorbent in the separation and purification of rutin and quercetin from Herba Artemisiae Scopariae combined with high‐performance liquid chromatography. Fourier transform infrared spectroscopy and field‐emission scanning electron microscopy were applied to characterize the deep eutectic solvent based molecularly imprinted polymers synthesized using different molar ratios of chalcone. The static and competitive adsorption tests were performed to examine the recognition ability of the molecularly imprinted polymers to rutin and quercetin. The ternary deep eutectic solvent consisting of formic acid/chalcone/methyltriphenylphosphonium bromide (1:0.05:0.5) had the best molecular recognition effect. After optimization of the washing solvents (methanol/water, 1:9) and eluting solvents (acetonitrile/acetic acid, 9:1), a reliable analytical method was developed for strong recognition towards rutin and quercetin in Herba Artemisiae Scopariae with satisfactory extraction recoveries (rutin: 92.48%, quercetin: 94.23%). Overall, the chalcone ternary deep eutectic solvent‐based molecularly imprinted polymer coupled with solid‐phase extraction is an effective method for the selective purification of multiple bioactive compounds in complex samples.     

Simultaneous determination of five triterpene acids in rat plasma by liquid chromatography–mass spectrometry and its application in pharmacokinetic study after oral administration of Folium Eriobotryae effective fraction

Folium Eriobotryae effective fraction (FEA), the extract of Folium Eriobotryae, had been used as anti‐hyperglycemia and anti‐hyperlipemia medicine in China. A previous study indicated that euscaphic acid, maslinic acid, corosolic acid, oleanolic acid and ursolic acid, the five structurally similar triterpene acids (containing two groups of structural isomers), are the major components of FEA. In the present study, we developed a specific and reliable LC‐MS method for simultaneous determination of the five triterpene acids in rat plasma, and further investigated their pharmacokinetic properties after oral administration of FEA. Following a simple sample preparation, chromatographic separation was achieved on a C₁₈ column with a mobile phase composed of methanol–0.1% ammonium acetate (80:20, v/v). Quantification was achieved by monitoring the selected ions at m/z 487.6 for euscaphic acid, m/z 471.5 for maslinic acid and corosolic acid, m/z 455.5 for oleanolic acid and ursolic acid and m/z 469.5 for internal standard. The method was validated to be specific, accurate and precise over the concentration ranges of 10–3000 ng/mL with limits of detections of 5 ng/mL for the five triterpene acids. Finally, the method was successfully applied to the pharmacokinetic study of the five structurally similar triterpene acids in rats after oral administration of FEA. Copyright © 2015 John Wiley & Sons, Ltd.     

紫外分光光度法测定艾叶中总黄酮含量

测定波长为290nm,以柚皮素为对照品,紫外分光光度法测定了艾叶中总黄酮含量。柚皮素在1—8μg/mL具有良好的线性关系,艾叶中总黄酮含量为1.186%,平均加标回收率为101.5%。该方法简便、快捷、准确、重现性好,可作为检测艾叶中总黄酮含量的一种好方法。     

Crystal growth of calcium oxalate induced by the extracts of Semen Plantaginis and Folium Pyrrosiae

The crystallization of calcium oxalate (CaOxa) in aqueous solutions of the extracts of Semen Plantaginis and Folium Pyrrosiae has been investigated, focusing on the inhibition mechanism of some herbs on stone formation. It has been shown that in the presence of extracts of above two herbs, calcium oxalate dihydrate (COD) crystals with typical morphologies of tetragonal bipyramids were obtained. This suggests that the extracts of Semen Plantaginis and Folium Pyrrosiae can promote the formation of thermodynamically unstable COD, and inhibit the formation of calcium oxalate monohydrate (COM), a major component of urinary stone. The formation mechanism of COD crystals induced by Semen Plantaginis and Folium Pyrrosiae is also discussed, indicating that the bioorganic molecules in the extracts of the herbs can induce the nucleation and growth of COD crystals. This study can help us make clear the inhibition mechanism of some herbs on stone formation that is in favor of the prevention and treatment of urolithiasis. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Fermentation characteristics and the dynamic trend of chemical components during fermentation of Massa Medicata Fermentata

As a representative of traditionally fermented Chinese medicine, Massa Medicata Fermentata (MMF) shows the functions of invigorating the spleen and stomach and promoting digestion, which plays an important role in the treatment of gastrointestinal diseases. The fermentation mechanism and the key factors that affect the quality of MMF have not been revealed yet, which has become an urgent issue that limits its clinical application. This article aims to systematically and comprehensively reveal the transformation of physical properties and the dynamic trend of chemical components including substrate components, volatile components, and lactic acid as anaerobic fermentation product during MMF fermentation. Along with obvious hyphae growth observed for MMF, the weight of MMF decreased, and the moisture and temperature increased. Through the quantified 14 components from substrate, ferulic acid increased from 45.53 ± 6.94 to 141.89 ± 78.40 μg/g, while glycosides and phenolic acids declined except caffeic acid. Also, within the 66 volatile components analyzed, alcohols and acids increased, while aldehydes and ketones decreased. Lactic acid was not detected in the fermentation substrate, but an apparent increase in lactic acid content was observed along with the increased fermentation days, resulting in 2.54 ± 0.15 mg/g on day 8. Based on the tested components, the fermentation process of MMF was discriminated into three distinct stages by principal component analysis, and an optimal fermentation time of four days was proposed. The results of this study will be of great significance to clarify the characteristics of fermentation and conduce to improving quality standards of MMF.     

艾叶挥发油的化学成分

采用水蒸气蒸馏法从艾叶中提取挥发油,试用不同类型的毛细管柱进行分析,找出最佳分析条件,共分离出59个蜂,用归一化法测定其相对含量,并用气相色谱－质谱法对化学成分进行鉴定,共鉴定了51个万分,占挥发油总成分的86％以上。     

艾纳香挥发油化学成分的气相色谱 -质谱分析

由黔产艾纳香（Blumea balsamifera DC.)的叶提取挥发油,分出结晶后的母液,用气相色谱－质谱进行定性分析和峰面积相对含量的测定,鉴定出41个化学成分;主要成分为L－龙脑、樟脑、β-石竹烯、桉叶油醇、古芸烯、芳樟醇等。     

高效液相色谱法同时测定忍冬中7种成分

建立了在不同时间段内转换使用不同波长同时测定忍冬花和叶中7种化学成分(绿原酸、咖啡酸、芦丁、木犀草苷、异绿原酸A、异绿原酸B、异绿原酸C)的高效液相色谱分析方法,同时应用该方法分析了忍冬花、忍冬老叶和新叶中成分含量的差异。色谱柱为Agilent Eclipse Plus C18(250 mm×4.6 mm, 5 μm);流动相为0.3%甲酸水溶液(A)和乙腈(B),梯度洗脱,流速1 mL/min;采用VWD紫外检测器转换波长(330 nm、350 nm)检测。应用所建立的方法测定忍冬新叶中绿原酸、木犀草苷含量分别为2.572%、1.498‰,均比药典中规定的含量高,有必要进一步的研究和开发利用。该方法准确、简便、灵敏度高,适用于忍冬中7种化学成分含量的同时测定和忍冬的质量控制及综合评价。     

基于稀疏主成分分析特征选择算法的山楂叶产地判别模型研究

为实现山楂叶产地的快速判别,提出一种基于稀疏主成分分析特征选择（SPCAFS）与支持向量机（SVM）建模的定性分析方法。采用近红外积分球漫反射光谱法采集6个产地共41批山楂叶123份样品的近红外光谱图,经数据预处理后,通过SPCAFS对代表性特征波段进行选择,并采用SVM建立山楂叶近红外产地判别模型。模型与连续投影（SPA）,正则化自表示（RSR）和稀疏子空间聚类（SSC）3种特征选择算法进行对比,以准确率、精确度和灵敏度作为评价标准,评估所提模型的预测性能。结果显示,SPCAFS的特征波段数相比于全波长建模从1 500减少到21,预测结果的准确率和精确度分别从78%、76%提升至97%、100%。同时,相比于SPA、RSR、SSC算法,准确率分别提升了6%、3%、3%,精确度分别提升了13%、10%、5%,模型的预测能力得到显著提升,基于SPCAFS的SVM判别模型可实现山楂叶南北产地的快速判别。     

代森锌在板蓝根和大青叶中的残留分析

采用顶空气相色谱法(火焰光度检测器)测定板蓝根、大青叶中代森锌的残留量。测定结果表明代森锌在0.1～5mg/kg范围内峰面积和进样量成良好的线性关系(R2=0.9985),回收率在80.6%～115.2%之间,变异系数在4.8%～9.0%之间,最低检出浓度为0.01mg/kg。该方法简便、快速、灵敏度高。