团状雪灵芝三种提取工艺的红外光谱跟踪分析

为了建立一种基于红外光谱跟踪分析的过程分析方法用于团状雪灵芝(AP)提取分离过程的宏观指导,从同一工艺不同提取物及不同工艺同一提取物两个方面,对三种提取工艺各四种提取物进行红外光谱跟踪测试,并对红外光谱及相应二阶导数谱进行了深入的对比分析研究。光谱分析结果显示,同一工艺的不同提取物具有明显不同的光谱吸收特征;不同工艺同一提取物的吸收特征总体相似,但彼此之间也存在明显的光谱差异。1 603和1 123cm-1的特征峰表明,提取法一中,黄酮类及其糖苷主要进入了酯提物,余者进入了醇提物。相反,方法二、三中,大部分黄酮类进入了醇提物,水提物中还存在微量黄酮苷。此外,根据2 850cm-1峰强可知,方法二酯提物中苷元及高级饱和烃基含量较高。类似的,1 066和2 927cm-1等特征吸收峰表明方法三的醇提物中糖苷及多糖含量较高。研究结果表明,AP组分在不同提取工艺中的迁移规律不尽相同,提取过程中的物质迁移信息可以通过各提取物红外光谱的跟踪分析进行记录和直观解析。红外光谱跟踪分析法是一种快速、有效、低碳、环保的过程分析方法,对于诸如AP等植物提取分离过程的质量控制或工艺优化具有宏观指导意义。     

Anti‐inflammatory bioactive equivalence of combinatorial components β‐carboline alkaloids identified in Arenaria kansuensis by two‐dimensional chromatography and solid‐phase extraction coupled with liquid–liquid extraction enrichment technology

Bioactive equivalent combinatorial components play a critical role in herbal medicines. However, how to discover and enrich them efficiently is a question for herbal pharmaceuticals researchers. In our work, a novel two‐dimensional reversed‐phase/hydrophilic interaction high‐performance liquid chromatography method was established to perform real‐time components trapping and combining for preparation and isolation of coeluting components. Arenaria kansuensis was taken as an example, and solid‐phase extraction coupled with liquid–liquid extraction as a simple and efficient method for enriching trace components, reversed phase column coupled with hydrophilic interaction liquid chromatography XAmide column as two‐dimensional chromatography technology for isolation and preparation of coeluting constituents, enzyme‐linked immune‐sorbent assay as bio‐guided assay, and anti‐inflammatory bioactivity evaluation for bioactive constituents. A combination of 12 β‐carboline alkaloids was identified as anti‐inflammatory bioactive equivalent combinatorial components from A. kansuensis , which accounts for 1.9% w/w of original A. kansuensis . This work answers the key question of which are real anti‐inflammatory components from A. kansuensis and provides a fast and efficient approach for discovering and enriching trace β‐carboline alkaloids from herbal medicines for the first time. More importantly, the discovery of bioactive equivalent combinatorial components could improve the quality control of herbal products and inspire a herbal medicine based on combinatorial therapeutics.     

A New Iridoid Glycoside and a New Iridoid from Pedicularis kansuensis f. aibiflora

A new iridoid glycoside 1 and a new iridoid 2 were isolated from the whole plant ofPedicularis kansuensis f. albiflora. Their structures were elucidated by spectroscopic methods.     

New Minor Cyclopeptides from Arenaria oreophila （Caryophyllaceae）

New minor cyclic peptides, named arenariphilin C 1 and arenariphilin D 2, were isolated from the whole plants of Arenaria oreophila (Caryophyllaceae). Their structures were determined as cyclo(Pro1-Pro2-Leu1-Leu2-Phe-Ser-Gly-Thr) and cyclo (Ser-Cys) on the basis of spectroscopic data, especially by two-dimension NMR (2D NMR) technologies.     

甘肃棘豆挥发性成分研究Ⅰ．精油成分分离与鉴定

草原毒草甘肃棘豆（ｏｘｙｔｒｏｐｉｓｋａｎｓｕｅｎｓｉｓｂｕｎｇｅ）全草经水蒸汽蒸馏得一种淡黄色半固体油状物。应用双柱分别进行ＣＧＣ／ＭＳ／ＤＳ分析和标准品对照，鉴定和初步鉴定了７７种组分，占全部峰面积的８１．２％，其中含量高于２％的有顺－法呢醇（ｃｉｓ－ｆａｒｎｅｓｏｌ）、月桂酸（ｌｉｕｒｉｃａｃｉｄ）、肉豆蔻酸（ｍｙｒｉｓｔｉｃａｃｉｄ）、１２－甲基肉豆蔻酸（ｍｙｒｉｓｔｉｃａｃｉｄ，１２－ｍｅｔｈｙｌ）、６，１０，１４－三甲基十五酮－２（２－ｐｅｎｔａｄｅｃａｎｏｎｅ，６，１０，１４－ｔｒｉｍｅｔｈｙｌ）、十九碳双烯醛（ｎｏｎａｄｅｃａｄｉｅｎｏｉｃａｌｄｅｈｙｄｅ），棕榈酸（ｐａｌｍｉｔｉｃａｃｉｄ）含量高达２８．１％。     

大孔吸附树脂预处理-HPLC法测定甘肃棘豆中苦马豆素含量

应用大孔吸附树脂为样品前处理技术,对甘肃棘豆中干扰苦马豆素含量测定的化合物进行选择性吸附除杂,以HPLC法测定样品中的苦马豆素含量.方法的平均回收率为92.81%(相对标准偏差为3.67%),日内和日间精密度分别为1.40%和3.98%,线性范围为0.022～0.730 mg/mL,方法检出限为0.010 mg/mL.方法可有效去除苦马豆素测定的干扰化合物,适用于甘肃棘豆中苦马豆素的含量测定.     

A New Flavonoid from Oxytropis kansuensis

Oxytropis kansuensis Bunge (Leguminosae) is a medicinal plant growing in southeast and northwest areas of China. It has been used as a folk medicine in China for treatment of cold and inflammation of carbuncle swelling, pain and different types of bleedin…     

A New Iridoid Glycoside and a New Iridoid from Pedicularis kansuensis f. albiflora

A new iridoid glycoside 1 and a new iridoid 2 were isolated from the whole plant of Pedicularis kansuensis f. albiflora. Their structures were elucidated by spectroscopie methods.     

Determination of Flavonoids Compounds of Three Species and Different Harvesting Periods in Crataegi folium Based on LC-MS/MS

Crataegi folium have been used as medicinal and food materials worldwide due to its pharmacological activities. Although the leaves of Crataegus songorica (CS), Crataegus altaica (CA) and Crataegus kansuensis (CK) have rich resources in Xinjiang, China, they can not provide insights into edible and medicinal aspects. Few reports are available on the qualitative and quantitative analysis of flavonoids compounds of their leaves. Therefore, it is necessary to develop efficient methods to determine qualitative and quantitative flavonoids compounds in leaves of CS, CA and CK. In the study, 28 unique compounds were identified in CS versus CK by qualitative analysis. The validated quantitative method was employed to determine the content of eight flavonoids of the leaves of CS, CA and CK within 6 min. The total content of eight flavonoids was 7.8–15.1 mg/g, 0.1–9.1 mg/g and 4.8–10.7 mg/g in the leaves of CS, CA and CK respectively. Besides, the best harvesting periods of the three species were from 17th to 26th September for CS, from 30th September to 15th October for CA and CK. The validated and time-saving method was successfully implemented for the analysis of the content of eight flavonoids compounds in CS, CA and CK for the first time.