安石榴苷的研究进展

安石榴苷是石榴皮多酚的主要成分,具有抗氧化、抗癌、抗菌、抗病毒、抗炎等多种药理学功效.本文作者主要对国内外关于安石榴苷的研究进行了综述,详细阐述了安石榴苷的结构、提取分离方法、含量测定、活性及代谢方式等研究进展,以期为安石榴苷的开发应用提供参考依据.     

响应面法优化石榴叶多酚闪式提取的工艺研究

为建立快捷、高效、绿色的石榴叶多酚的提取工艺,通过单因素实验确定其主要影响因素,在单因素实验的基础上利用响应面法进行分析,确定提取石榴叶多酚的最佳提取条件为:乙醇浓度58%、料液比1∶9 (g/mL),提取时间4 min,在此条件下石榴叶多酚的理论提取量为:29.37 g GAE/100 g,实际提取量为:29.12 g GAE/100 g.     

莲藕中儿茶素的高效液相色谱分析

儿茶素属于环烷醇类化合物,为多酚中的一种单体化合物。研究表明多酚类化合物具有延缓衰老、抗肿瘤、抑菌、防紫外线辐射、抗氧化等生物功能。有关茶叶、儿茶、苹果中儿茶素的高效液相色谱(HPLC)分析的研究较多,但对莲藕中儿茶素的分析未见报道。本文确定了莲藕中儿茶素HPLC分离的条件,建立了莲藕中儿茶素定性定量的方法。本方法有较好的重现性。     

刺五加叶中黄酮类化合物的结构鉴定

利用电喷雾质谱发现刺五加叶中存在4种黄酮类化合物,进一步分离得到其中的两种,经核磁质谱鉴定,一种为槲皮甙(槲皮素－3－O－α－L－鼠李糖),另一种为金丝桃甙(槲皮素－3－O－β-D－半乳糖).其余两种难以分离的黄酮甙经电喷雾多级串联质谱分析,初步推断为槲皮素和芦丁(槲皮素－3-O－芦丁糖).以上4种均为黄酮醇类化合物,除金丝桃甙外,其它3种为刺五加叶中尚未见报道的黄酮类成分.     

水母雪莲化学成分的研究（Ⅱ）

前文已报道从水母雪莲(Saussurea Medusa Maxim)中分得4种黄酮甙,本文报道另外6种化合物的分离和鉴定。 1 化合物Ⅰ—Ⅳ物化性质及分离鉴定 1.1 化合物Ⅰ 黄色结晶,m.p.:249～251℃,水解所得甙元鉴定为木樨草素,纸层析检出鼠李糖和葡萄糖。MS(FAB):m/z 595(M~++1),287(M~++H-葡萄糖基-鼠李糖)。化合物I与木樨草素的~(13)C NMR比较,C_6、C_8、C_(10)分别向低场位移1.1、1.0、1.8 ppm,而C,向高场移动     

液相色谱-电喷雾电离质谱与电子轰击质谱联用筛选百合中的甾体皂甙

 利用高效液相色谱 电喷雾电离质谱联用仪 (HPLC/ESI MS)、电子轰击质谱 (EI MS)和半制备型高效液相色谱 ,从卷丹百合中筛选出了两种甾体皂甙 ,其中一种为含有 3个糖基与提果皂甙元的甾体皂甙 ,另一种为含有 3个糖基和薯蓣皂甙元的甾体皂甙。结果表明 :在线的HPLC/ESI MS能够准确快速地提供糖甙类化合物的分子质量和糖链部分的有益信息 ,但对甙元部分提供的信息极少 ;离线的EI MS只需极少量 (1mg～ 2mg)的纯品就能准确地提供甙元部分的有益信息 ,但很难获得糖甙的分子离子峰与糖链部分的信息 ,两者有机地结合起来能快速地从植物中筛选甾体皂甙。     

金纳米棒荧光探针应用于多酚化合物检测新方法

以金纳米棒为荧光探针,在20％甲醇(pH 5.0～6.0)介质中,以植物多酚化合物芒果苷、瑞香素和白藜芦醇为检测对象,建立了3种植物多酚的灵敏、简便、快速检测新方法.多酚化合物基于其与金纳米棒表面的十六烷基三甲基溴化铵(CTAB)分子间的疏水作用而在金纳米棒表面富集,同时使金纳米棒在719 nm处的荧光强度减弱,在一定范围内多酚化合物的浓度与金纳米棒荧光强度成正比,其检出限分别为5.0×10-8、8.0×10-8、2.0×10 -7mol/L.     

高效液相色谱-质谱甄别七种化学战剂相关化合物

建立了高效液相色谱-质谱(HPLC-MS)甄别7种化学战剂相关化合物的分析方法,采用C18柱分离了包括酸性、中性和碱性在内的7种化学战剂相关化合物,选择离子监测法(SIM)测定这7种化合物的检出限在0．01—1mg/L之间。利用HPLC～APCI^ MS测定了4种土壤中的双(2-羟乙基)亚砜,此方法回收率大于93％,相对标准偏差(RSD)小于4％.     

常见植物多酚化合物的介绍

从物质结构、医药功能、提取与合成方法等角度对没食子酸、白藜芦醇、槲皮素和姜黄素等4种常见植物多酚化合物及其衍生物展开介绍。这些植物多酚化合物都具有抗氧化、抗菌、抗肿瘤等生物活性,可广泛应用于医药、农业、食品添加剂等行业。     

长毛风毛菊化学成分的研究

从长毛风毛菊地上部分分离得到9种化合物,经化学和光谱方法鉴定它们为:东茛菪素(E_1)、伞形花内酯(E_2)、柯伊利素(E_3)、木犀草素(E_4)、牛蒡子甙(B_1)、茵芋甙(B_2)、木犀草素-7-O-β-D-葡萄糖甙(B_4)、紫丁香甙(B_5)和一种新的倍半木脂素(Sesquilignan)(E_5),暂定名为Saussol.     

Determination of hydrolyzable tannins in the fruit of Terminalia chebula Retz. by high-performance liquid chromatography and capillary electrophoresis

A RP-HPLC method for determining fourteen components (gallic acid, chebulic acid, 1,6-di-O-galloyl-D-glucose, punicalagin, 3,4,6-tri-O-galloyl-D-glucose, casuarinin, chebulanin, corilagin, neochebulinic acid, terchebulin, ellagic acid, chebulagic acid, chebulinic acid, and 1,2,3,4,6-penta-O-galloyl-D-glucose) in the fruit of Terminalia chebula Retz. is described. The separation was achieved within 80 min using a binary gradient with mobile phases consisting of a pH 2.7 phosphoric acid solution and an 80% CH3CN solution. Capillary electrophoretic analyses were also attempted, and it was found that CZE (25 mM Na2B4O7, 5 mM NaH2PO4, pH 7.0) was an efficient method for the separation of gallotannins, while an MEKC method (25 mM Na2B4O7, 5 mM NaH2PO4, 20 mM SDS, pH 7.0, and 10% acetonitrile) provided a better separation for most of the tannins examined. The HPLC and CE methods developed were both successfully applied to the assay of tannins in commercial samples of Chebulae Fructus.     

Carbon molecular sieve based micro‐matrix‐solid‐phase dispersion for the extraction of polyphenols in pomegranate peel by UHPLC‐Q‐TOF/MS

A rapid, simple, and efficient sample extraction method based on micro‐matrix‐solid‐phase dispersion (micro‐MSPD) was applied to the extraction of polyphenols from pomegranate peel. Five target analytes were determined by ultra‐HPLC coupled with Q‐TOF/MS. Carbon molecular sieve (CMS) was firstly used as dispersant to improve extraction efficiency in micro‐MSPD. The major micro‐MSPD parameters, such as type of dispersant, amount of dispersant, grinding time, and the type and the volume of elution solvents, were studied and optimized. Under optimized conditions, 26 mg of pomegranate peel was dispersed with 32.5 mg of CMS, the grinding time was selected as 90 s, the dispersed sample was eluted with 100 μL of methanol. Results showed that the proposed method was of good linearity for concentrations of analytes against their peak areas (coefficient of determination r² > 0.990), the LOD was as low as 3.2 ng/mL, and the spiking recoveries were between 88.1 and 106%. Satisfactory results were obtained for the extraction of gallic acid, punicalagin A, punicalagin B, catechin, and ellagic acid from pomegranate peel sample, which demonstrated nice reliability and high sensitivity of this approach.     

高效液相色谱法测定烟火药剂中的没食子酸

建立了烟火药剂中没食子酸的高效液相色谱检测方法。采用ZorbaxEclipse XDB-C18色谱柱(4.6×150 mm)分离,以甲醇-0.1%冰乙酸水溶液为流动相,梯度洗脱,流速1.0 mL/min;测定温度为25℃;采用紫外检测器检测,检测波长为274 nm。没食子酸的质量浓度在0.5~20μg/mL时与色谱峰面积之间线性关系良好(相关系数r=0.9999);对烟火药剂样品进行3个不同浓度水平的添加回收,回收率为90.8%~100.2%,相对标准偏差(RSD)为1.2%~6.4%。     

高速逆流色谱法分离制备中药诃子中的没食子酸

利用高速逆流色谱法从100 mg诃子醇提物中一次性分离制备得到8.6 mg没食子酸。通过分析型高速逆流色谱对5种溶剂系统进行筛选,确定以正己烷-乙酸乙酯-甲醇-水(体积比为1:5:1:5)为两相溶剂体系并放大到制备型上,以上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2 mL/min、检测波长254 nm的条件下进行分离制备,获得4个分离峰(组分Ⅰ、Ⅱ、Ⅲ、Ⅳ)。经高效液相色谱检测,按照面积归一法计算,其中组分Ⅲ的纯度达96.40%。经电喷雾电离质谱分析,并结合与没食子酸标准品的高效液相色谱测定结果的对比,确定组分Ⅲ为没食子酸。该方法简便、快速、重复性好,适合于诃子中没食子酸的分离制备。     

Analysis of phenolic constituents of biological interest in red wines by high-performance liquid chromatography

We describe a reversed-phase HPLC method that uses gradient elution and diode array detection to determine four biologically active phenolic constituents of red wines: gallic acid, trans-resveratrol, quercetin and rutin. The method permits direct injection without sample pre-treatment. ODS Hypersil served as the stationary phase; the gradient was formed by acetic acid, methanol, and water. Each analysis required an equilibration period of 10 min and a run time of 50 min for completion. Previously, total phenols were analysed according to the Folin-Ciocalteu method, using gallic acid as the standard, and the results are given as gallic acid equivalent.     

Quantitative and qualitative determination of Liuwei Dihuang tablets by HPLC-UV-MS-MS

A method is developed for the analysis of allantoin, gallic acid, dihydromelittoside, loganin, paeoniflorin, benzoylpaeoniflorin, and paeonol in Liuwei Dihuang tablets by high-performance liquid chromatography (HPLC)-UV-mass spectrometry (MS)-MS. Gradient elution with methanol-acetonitrile-water-formic acid solvent system is employed in the HPLC-electrospray ionization-MS study. The positive-ion ESI mode is suitable for these compounds. The peaks of gallic acid, loganin, dihydromelittoside, paeoniflorin, benzoylpaeoniflorin, and paeonol are identified by their mass spectra and the fragments of their MS-MS spectra. Allantoin, gallic acid, loganin, paeoniflorin, and paeonol are simultaneously determined by UV detection at 210 nm for quantitative purposes.     

HPLC法测定怀菊花中没食子酸的含量

为建立HPLC法测定怀菊花中没食子酸含量测定方法,采用Agilent C18柱(150 mm×4.6mm,5μm),以V(甲醇)+V(超纯水+0.1%磷酸)=25+75为流动相,流量:0.5 mL·min1;柱温为25℃,检测波长:258 nm;进样量:10μL,进行测定。结果表明,回归方程为y=3.054 2 x-2.207 1,r2=0.999 1(n=6),线性范围0～20μg,平均回收率97.28%,RSD为3.39%。样品中没食子酸质量分数为3.17 mg/g。方法快速、简便、准确、重现性较好,结果可靠,可为怀菊花中没食子酸的质量评价提供依据。     

Development of analytical method for the quality control of the fruit bark of Punica granatum L. (pomegranate) and antichemotatic activity of extract and rich fraction in punicalagins

Pomegranate is of current interest owing to the existing potential for industrial uses of fruit peels. This includes its availability as a raw vegetable material, a byproduct that constitutes residue in the use of the species and is recognized as a functional product, and beneficial health properties, as will be demonstrated in the studies cited. Therefore, it is necessary to ensure its effectiveness and safety. Toward this end, the aim of this study was to develop and validate an analytical method for the separation and quantification of total punicalagin present in the bark of the fruit of Punica granatum by HPLC. Purity tests such as water determination and total ashes were also performed. The ability of the extract and enriched fraction of punicalagin to inhibit leukocyte migration in vitro was determined by the Boyden's chamber method. The developed HPLC method demonstrated good separation and quantification of the punicalagin α and β anomers. The method is efficient and reliable, and can ultimately be used for the analysis of the extract of pomegranate. The crude extract and the fraction of punicalagins significantly inhibited leukocyte migration at concentrations of 1 and 10 μg/mL in relation to the negative control, indicating potential antichemotactic action.     

Simultaneous determination of bergenin and gallic acid in Bergenia ligulata wall by high-performance thin-layer chromatography

A simple and reproducible high-performance thin-layer chromatographic method was developed for the simultaneous determination of bergenin and gallic acid in Bergenia ligulata. Water and methanol were used as the extracting solvents. The concentrations of bergenin and gallic acid in both of these solvents were found to be almost the same. The method involves separation of the components by thin-layer chromatography on a precoated Silica Gel 60 F254 plate with a solvent system of ethyl acetate-formic acid-acetic acid-water (100 + 11 + 11 + 27). The sensitivity of the method for bergenin was 0.30 microg, whereas for gallic acid it was 0.25 microg. The proposed method is precise and sensitive and can be used for the detection, monitoring, and simultaneous quantification of bergenin and gallic acid in B. ligulata.     

A rapid densitometric method for simultaneous quantification of gallic acid and ellagic acid in herbal raw materials using HPTLC

Gallic acid and ellagic acid are two widely occurring phenolic compounds of plant origin, to which many biological activities including anticancer and antiviral activity have been attributed. A simple HPTLC method has been developed for the simultaneous quantification of gallic acid and ellagic acid. The method was validated for precision, repeatability, and accuracy. Instrumental precision was found to be 0.083 and 0.78, and the repeatability of the method was found to be 1.07 and 1.50 (% CV) for gallic acid and ellagic acid, respectively. The accuracy of the method was checked by a recovery study conducted at two different levels and the average percentage recovery was found to be 101.02% for gallic acid and 102.42% for ellagic acid. The above method was used for the quantification of gallic acid and ellagic acid content in seeds of Abrus precatorius Linn., whole plant of Phyllanthus maderaspatensis Linn., and flowers of Nymphaea alba Linn. The proposed HPTLC method for the simultaneous quantification of gallic acid and ellagic acid was found to be simple, precise, specific, sensitive, and accurate and can be used for routine quality control of herbal raw materials and for the quantification of these compounds in plant materials.