HPLC法测定菊花及其炮制品中主要成分的含量

目的:建立检测菊花及其炮制品种主要成分的方法,并对三批菊花及其炮制品中的主要成分绿原酸(C16H18O9)、木犀草苷(C21H20O11)、异绿原酸A(C25H24O12)进行含量测定。方法:色谱柱Agilent XBD C18(4.6 mm×250 mm,5.0μm),流动相乙腈/0.1%磷酸,流速1.0 m L/min,柱温25℃,检测波长348 nm。结果:三种化合物的分离度较好,理论塔板数较高,绿原酸:A=8.278 71C+4.935 05,R=0.999 9(n=7),浓度范围为8.656~86.56μg/m L;木犀草苷:A=15.866 45C-2.036 02,R=0.999 9(n=7),浓度范围为4.16~41.60μg/m L;异绿原酸A:A=8.514 90C+1.2142 8,R=1.0(n=7),浓度范围为18.92~189.20μg/m L,三种化合物的峰面积和浓度有良好的线性关系。结论:本方法能够准确快速地对菊花及其炮制中,主要成分进行定量分析,具有简便、稳定、准确等特点。     

山豆根主要活性成分含量及影响因素研究进展

药用植物有效成分及其含量是评价药材质量的关键指标和发挥临床疗效的物质基础。山豆根是我国重要的药用植物之一,山豆根碱是山豆根的主要活性成分和发挥药效及毒性作用的主要物质基础。由于野生资源濒临枯竭,人工种植成为保障市场需求的主要途径。为此,笔者整合分析近年来山豆根植物根、茎和叶的主要活性成分、含量特征,重点论述了光照条件、水分含量、养分特征、种群密度和微生物等环境因子对有效活性成分含量影响。综合当前人工栽培山豆根立地选择、种植密度和管护等栽培技术,分析相关研究存在的问题及瓶颈,以期为山豆根资源高效利用提供参考。     

山楂核干馏油GC-MS主要成分分析及含量测定

本研究目的在于建立气相色谱-质谱联用法(GC-MS)分析山楂核干馏油中挥发油、脂溶性成分以及气相色谱法(GC-FID)同时测定山楂核干馏油中活性成分的定量分析方法。采用GC-MS法对山楂核干馏油化学成分进行分析,共分析出62种化学成分,用峰面积归一化法测定各成分的相对百分含量,含量最高的化合物为醛类,占总量的55.96%。以GC-FID法同时测定山楂核干馏油中的主要成分的含量(糠醛、愈创木酚、2,6-二甲基苯酚、2-甲基苯酚、苯酚、2-甲氧基-4-甲基苯酚、2,6-二甲氧基苯酚、四氯愈创木酚、1,2,3-三甲氧基苯、3,4,5-三甲氧基甲苯),测得加样回收率范围为100.06%~102.44%,RSD范围为2.98%~4.57%。本方法准确、简便、重复性好,为山楂核干馏油制剂的内在质量控制及提升废弃物山楂核循环利用价值提供依据。     

不同产地野菊花中黄酮类成分含量的HPLC分析

野菊花为菊科(Compositae)植物野菊[Dendranthema indicum (L.) Des Moul.]的头状花序,具有清热解毒和疏风散热等功效.黄酮类化合物为野菊花最主要的有效成分之一,最早从野菊花中分离出的黄酮类化合物为木犀黄酮苷,此后相继得到刺槐素、木犀草素、芹菜素和蒙花苷等黄酮类化合物,以蒙花苷和木犀草素含量最高,其中蒙花苷含量是野菊花药材的主要质量检测指标[1].     

基于HPLC指纹图谱与多成分含量测定结合化学计量学的玉屏风散质量评价

建立玉屏风散HPLC指纹图谱结合化学计量学的方法对其进行分析,并测定其中11种成分的含量,为玉屏风散质量控制提供科学依据.采用Shimadzu Inertsil ODS-2 C18(250mn× 4.6 mm,5μm)色谱柱,以乙腈-水为流动性进行梯度洗脱,流速1.0 mL/min,柱温30℃,检测波长230 nm.1...     

不同产地铁皮石斛主要成分及甲醇提取物HPLC指纹图谱研究

本文采用紫外分光光度法、高效液相色谱法(HPLC)测定铁皮石斛中总黄酮、多糖、柚皮素、石斛酚的含量,同时运用HPLC法建立霍山铁皮石斛及其他产地铁皮石斛甲醇提取物HPLC指纹图谱并聚类分析。实验结果显示不同产地铁皮石斛的主要化学成分含量存在差异,5批霍山铁皮石斛的总黄酮、柚皮素、石斛酚含量较高,多糖含量较低。建立了霍山铁皮石斛的共有指纹图谱模式,5批霍山铁皮石斛具有极高的相似度,在92.6%~94.8%之间,浙江临安、浙江乐清、江苏盐城、云南昆明所产的铁皮石斛相似度在17.5%~41.5%之间。5批来自安徽霍山的铁皮石斛共有峰总面积较高,为9 827.40~14 102.28。其他产地铁皮石斛的共有峰面积在730.27~4 206.20之间,明显低于霍山铁皮石斛。聚类分析结果可分为两大类,安徽霍山为一类,其他产地为一类。霍山铁皮石斛与其他产地铁皮石斛存在一定差异,且小分子成分含量较高。上述结果为进一步研究霍山铁皮石斛化学成分提供参考,为铁皮石斛品质鉴别、质量控制及资源的综合利用提供实验依据。     

黄芪百合颗粒HPLC指纹图谱及多指标成分定量研究

建立黄芪百合颗粒(HBG)的HPLC指纹图谱,并进行多指标成分定量测定,为其质量评价提供依据。采用Agilent Eclipse Plus C18色谱柱(4. 6 mm×250 mm,5μm),以0. 2%甲酸溶液(A)-乙腈(B)为流动相,梯度洗脱(0~10 min,5%→10%B; 10~35 min,10%→30%B; 35~40 min,30%B; 40~50 min,30%→60%B; 50~60min,60%→5%B),流速1. 0 mL/min,250、260、290、330 nm多波长切换,柱温30℃,建立了HBG的指纹图谱,共确定28个共有峰,10批HBG指纹图谱中样品间相似度均大于0. 99。通过与对照品比较指认出其中6个共有峰并分别进行了定量分析,6个共有峰分别为毛蕊异黄酮葡萄糖苷(15号峰)、橙皮苷(18号峰)、芒柄花苷(21号峰)、毛蕊异黄酮(23号峰)、芒柄花素(25号峰)、川陈皮素(26号峰)。所建立的HPLC指纹图谱和含量测定分析方法可用于HBG的质量评价。     

金蝉花核苷类成分的LC-MS定性分析与HPLC含量测定

本文采用高效液相色谱-质谱联用法定性分析金蝉花中核苷类成分,并建立了高效液相色谱法同时测定6种核苷类成分含量的方法。结果定性分析出金蝉花中13种核苷类成分,腺嘌呤、尿苷、肌苷、鸟苷、腺苷和N6-(2-羟乙基)腺苷在2.34～18.67、4.77～38.13、3.48～27.87、1.13～9.07、4.76～38.04、2.84～22.76μg/mL范围内呈良好的线性关系(r0.999 1),平均加样回收率为97.32%～102.37%,且精密度、重复性、稳定性良好,可用于金蝉花中主要核苷类成分的同时测定;不同产地的金蝉花中核苷类成分含量存在差异,安徽大别山和江苏句容的6种核苷类总量相对较高,浙江天目山、安徽宣城和福建三明相对较低;不同部位的金蝉花样品中,腺嘌呤、尿苷、肌苷、鸟苷、腺苷在子实体中含量均高于菌核,而N6-(2-羟乙基)腺苷则在菌核中含量较高。以上结果可为金蝉花的质量控制及深入开发利用提供参考。     

HPLC测定莪术油葡萄糖注射液中四种成分的含量

采用HPLC法测定了莪术油葡萄糖注射液中四种成分(莪术二酮、莪术醇、牻牛儿酮、呋喃二烯)含量。本法以十八烷基硅烷键合硅胶为填充剂,流动相为甲醇-水(85∶15 V/V),流速为0.8mL/min,柱温:30℃,检测波长为215nm。在该色谱条件下,分别建立莪术二酮、莪术醇、牻牛儿酮、呋喃二烯的线性回归方程。结果表明,该法的精密度、重复性、稳定性良好(RSD<2.0%),平均回收率均大于96%(RSD<3.0%,n=5),通过测定得到莪术油葡萄糖注射液中四种主分的含量分别为67,26,20,45μg/mL。HPLC法准确、可靠、重复性良好,可用于莪术油葡萄糖注射液的质量控制。     

HPLC法同时测定苍耳类药材中酚酸及蒽醌类成分的含量

建立HPLC同时测定苍耳子、苍耳草药材中绿原酸、新绿原酸、原儿茶醛、原儿茶酸、隐绿原酸、咖啡酸、1,3-二咖啡酰奎宁酸、阿魏酸、3,4-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、4,5-二咖啡酰奎宁酸、芦荟大黄素、大黄素及大黄酚含量的方法。采用Agilent ZORBAX SB-C18色谱柱(250×4.6 mm,5μm),以甲醇(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,流速1.0 m L/min,柱温35℃,检测波长254 nm,进样量10μL。14种成分的浓度与峰面积的线性关系良好(r0.9931);加样回收率为97.18%~101.09%。苍耳类药材中酚酸和蒽醌类14种成分的含量存在差异,其中绿元素、原儿茶酸含量较高,芦荟大黄素、大黄素、大黄酚含量较低。该方法简单、准确,重现性较好,可用于苍耳类药材内在质量的评价和控制。     

Chemical constituents from Melodinus cochinchinensis (Lour.) Merr. and their chemotaxonomic significance

A phytochemical investigation on the twigs and leaves of Melodinus cochinchinensis (Lour.) Merr. resulted in the isolation and identification of 22 compounds, including seven sesamin-type lignans (1–7), three pentacyclic triterpenes (8–10), one anthraquinone (11), one flavanone (12), two phenolic compounds (13 and 14), five aspidosperma-type indole alkaloids (15–19), and three eburnan-type indole alkaloids (20–22). The structures of these compounds were elucidated by means of spectroscopic analysis, including HREIMS together with 1D and 2D NMR experiments, and comparison with reported data. Among them, compounds 1/4, 2/5, and 3/6 are three pairs epimers at C-7''. Compounds 1–6, 8 and 11 were firstly isolated from the family Apocynaceae, whereas 17 was isolated from Melodinus species for the first time. Compound 8 was only found in Juglans hopeiensis, while 11 was only found in roots of Rubia cordifolia. Compounds 1–6, 8, 11 and 15–22 could be considered as chemotaxonomic markers for M. cochinchinensis. Furthermore, the chemotaxonomic significance and distribution of these isolates in Melodinus genus are discussed in detail.     

Phytoconstituents from the leaves of Dracaena cochinchinensis (Lour.) S. C. Chen

Five flavonoids, four feruloyl amide derivatives, pinoresinol, lanost-9-en-3β-ol and three steroids from the leaves of Dracaena cochinchinensis (Lour.) S. C. Chen. Of these, compound 4 was identified as a new homoisoflavanone. This publication is the first reported purification of compounds 3, 4, 6–12 from D. cochinchinensis. We also indicate the chemotaxonomic importance of these metabolites.     

高效液相法测定蜂蜜中甘油的含量

建立了以混合溶剂直接提取测定蜂蜜中甘油含量的方法.采用ZORBAX Carbohydrate a-nalysis(4.6 mm×250 mm 5-Micro)色谱柱,以乙腈/水(80:20,v/v)为流动相,示差检测器,使用乙腈/甲醇/水混合作为溶剂快速检测甘油.结果表明,应用此法的甘油浓度在10.0 mg/L～250...     

Angiotensin II-induced increase in inositol 1,4,5-trisphosphate in cultured rat mesangial cells: evidence by refined high performance liquid chromatography

Angiotensin II-induced change in inositol phosphates were studied in cultured rat mesangial cells prelabeled with [3H]myo-inositol. By using anion-exchange high performance liquid chromatography, we could analyzed the change in inositol mono-, bis-, and tris-phosphate more rapidly and easily with higher resolution than the previously reported methods. Angiotensin II rapidly increased inositol 1,4,5-trisphosphate and inositol 1,4-bisphosphate within 15 sec, followed by an increase in inositol 1-monophosphate at 30 sec. Angiotensin II-induced increases in inositol phosphates were dose-dependent and completely blocked by saralasin. These results indicate that angiotensin II induces the production of inositol phosphates including inositol 1,4,5-trisphosphate, an intracellular Ca2+-releasing factor, in cultured rat mesangial cells.     

Isolation and some properties of a serine protease from the fruits of Cudrania cochinchinensis (Lour.) Kudo et Masam

An endopeptidase (Cudrania protease) with a molecular mass of 76 kDa has been purified from the fruits of Cudrania cochinchinensis (Lour.) Kudo et Masam. The enzyme was stable between pH 6 and 10 at 30 degrees C for 60 min. The enzyme activity was inhibited by diisopropyl fluorophosphate, chymostatin, and aprotinin, but not by EDTA or pepstatin. These results indicated that the enzyme was a serine protease.     

HPLC法测定牙膏中柚皮苷的含量

建立了高效液相色谱测定牙膏中柚皮苷含量的方法。采用的色谱条件:Hypersil BDS C18色谱柱(250 mm×4.6 mm,5μm);柱温为40℃;以水(A相)和乙腈(B相),梯度洗脱程序为:0～15 min,10%～100%B;流速为1.0 mL/min;检测波长为283 nm;进样量为20μL。结果表明,柚皮苷的质量浓度在14.55～116.40μg/mL范围内与峰面积呈良好的线性关系(r=0.9999),平均加标回收率为97.56%。该方法稳定、准确,重现性好,可作为牙膏中柚皮苷的含量测定和质量控制方法。     

Determination of methylputrescine oxidase by high performance liquid chromatography

N-Methyl-Δ¹-pyrrolinium chloride, the product of the title enzyme, was synthesized by methylation of aminobutyraldehyde diethylacetal followed by acidic cleavage. After purification to homogeneity, it was characterized by NMR and UV spectroscopy. The compound had an absorption maximum at 210 nm; previous data indicating a maximum at 267 nm were shown to arise from an impurity. An HPLC method for the assay of N-methylputrescine oxidase from plant material was developed based on the separation of N-methyl-Δ¹-pyrrolinium chloride on a cation exchange column and direct detection at 210 nm. The enzyme activity was measured in the protein fraction extracted from plant roots and treated by gel filtration on disposable PD 10 columns. A K_m value of 1.9 mM was determined for methylputrescine and the enzyme from tobacco roots. The enzyme activities from N. tabacum and Datura stramonium were compared.     

Analysis of apolipoproteins in high density lipoproteins by high performance liquid chromatography

A simple and rapid method for the analysis of apolipoproteins in high density lipoprotein (HDL) by high performance liquid chromatography (HPLC) has been developed (Kinoshita et al. (1983) J. Biochem. 94, 615-617). With this method, using a sodium phosphate buffer containing 0.1% sodium dodecyl sulfate (SDS) as an eluent, apolipoproteins can be analyzed from a very small amount of HDL fraction without delipidation using organic solvents. Separation profiles of apolipoproteins by this method were examined using several techniques. The elution pattern monitored by A280 can give precise quantitative as well as qualitative information about size-distribution of apolipoproteins, except for the apo C group. Moreover, separation of apo E from apo A-I was found to be improved by column elongation.