3种绿绒蒿挥发油化学成分的GC-MS分析

目的 分析全缘叶绿绒蒿、五脉绿绒蒿和多刺绿绒蒿挥发油的化学成分.方法 采用水蒸气蒸馏法获得挥发油,经GC-MS技术结合计算机检索对其化学成分进行分离和鉴定,用色谱峰面积归一化法计算各组峰的相对含量.结果 从全缘叶绿绒蒿、五脉绿绒蒿和多刺绿绒蒿的挥发油中分别鉴定了25,42和53个化合物,占其各自总量的80.76%,73.34%和76.10%.结论 3种绿绒蒿挥发油化学成分存在一定程度的差异,但其主要成分都为酯类物质

HPLC法测定野生与栽培藏药麻花艽中4种环烯醚萜苷类成分的含量

目的：对野生和栽培藏药麻花艽中龙胆苦苷、落干酸、獐牙菜苦苷和獐牙菜苷4种苦苷类成分进行高效液相色谱的含量测定，并比较分析它们之间的差异。方法：采用Eelipse XDB-C_8色潜柱(4.6 mm*150 mm，5 μm)，流动相A为95％乙腈水溶液，B为5％乙腈(含10 mmol•L~(-1)的甲酸)水溶液，A在0-20min内比例由0-100％进行线性洗脱，流速1.0 mL•min~(-1)，检测波长240 nm，柱温30℃。结果：4种成分均达到基线分离，龙胆菁苷、落干酸、獐牙菜苦苷、獐牙菜苷的线性范围分别为0.60～19•20μg(r=0.9999)，0.24～7.68μg(r=O.9999)，0.38-12.02μg(r=O.9999)，0.05～1.66μg(r=0.9999)；回收率分别为99.73％，98.13％，98.45％，96.22％。结论：栽培藏药麻花艽中苦苷类成分的含量已经接近或超过野生种的水平，可初步代替野生药材人药。

唐古特白刺籽油的超临界CO_2流体萃取及GC／MS分析

利用超临界CO_2萃取唐古特白刺籽油，并对籽油进行了GC／MS分析。实验确定的最佳超临界CO_2流体萃取条件是:萃取温度45℃，萃取压力20 MPa，CO_2流量为35-40 kg／h，萃取时间120min，在此条件下白刺籽油的萃取率为15.11％。利用GC／MS对白刺籽油分析，发现其不饱和脂肪酸的相对含量高达93.37％。比较了超临界CO_2萃取白刺籽油油样和石油醚萃取白刺籽油油样的理化性质，发现超临界CO_2流体萃取的籽油质量优于传统溶剂萃取的籽油。

HPLC测定刺芒龙胆不同部位中3种有效成分的含量

目的：建立反相高效液相色谱法同时测定刺芒龙胆植物不同部位落干酸、獐牙菜苦苷、龙胆苦苷的含量。方法：采用ZORBAX SB-C18（250mm×4．6mm，5μm）色谱柱，流动相为甲醇-水（含0．04％磷酸）的比例25：75，流速1mL·min^-1，检测波长238nm，柱温30℃。结果：3种成分均达到基线分离，落干酸、獐牙莱苦苷、龙胆苦苷的线性范围分别为0．039～1．56μg（r=0．9998），0．0725～1．45μg（r=0．9999），0．061～1．225μg（r=0．9997）；回收率为101．3％（RSD=2．6％），98．7％（RSD=3．1％，99．6％（RSD=1．2％）。结论：测定方法快速，结果准确、可靠。

SPE-HPLC法测定藏药能安均宁胶囊中胡椒碱的含量

目的建立能安均宁胶囊(主要由北寒水石,石榴子,荜茇等组成)中胡椒碱含量的测定方法.方法采用SPE-HPLC法,使用Kromasil C18柱,胡椒碱流动相为甲醇-水(77∶23);检测波长为343nm.结果胡椒碱平均回收率为99.07%,RSD%=2.43%(n=3).结论该方法简便、准确、重现性好,可以用作能安均宁胶囊质量控制.

西藏产两种岩白菜中岩白菜素的HPLC测定

建立测定了岩白菜中岩白菜素含量的方法.色谱柱:Waters C18柱(5 μm×3.9 mm×150 mm),流动相:甲醇∶水∶磷酸=20∶80∶0.1,流速为1.0 mL/min,检测波长275 nm,AUFS 0.01,柱温为室温.结果表明,岩白菜素在0.16～0.08 μg有良好线性关系,r=0.999 2,平均回收率为98.14%,RSD为1.12%.本方法是测定岩白菜中岩白菜素含量的快速、简便、准确可靠的定量方法.

HPLC法测定獐牙菜及其近缘植物中4种有效成分的含量

目的:建立反相高效液相色谱法同时测定獐牙菜及其近缘植物中番木鳖酸、獐牙菜苦苷、龙胆苦苷、芒果苷的含量。方法:采用ZORBAX SB—C18(250 mm×4.6mm,5μm)色谱柱,以流动相甲醇和水(含0.04%磷酸)的比例在0-24 min内由22:78至38:62线性梯度洗脱,流速1 mL•min～1,检测波长254 nm,柱温30℃。结果:4种成分均达到基线分离,番木鳖酸、獐牙菜苦苷、龙胆苦苷、芒果苷的线性范围分别为0.05—6.25μg(r=0.9999),0.0095—2.9 μg(r=0.9998),0.0486—2.56μg(r=0.9999),0.0056—2.8μg(r=0.9998);回收率为102%(RSD=4.4%),97.7%(RSD=4.3%),99.5%(RSD=3.5%),103%(RSD=1.1%)。结论:方法测定快速,结果准确、可靠。

藏药秦艽、麻花艽中落干酸和龙胆苦甙的HPLC法含量测定

应用反相高效液相色谱法同时测定藏药秦艽、麻花艽中落干酸、龙胆苦甙含量.并比较了加热回流提取及超声提取两种方法对分析结果的影响.还测定了两种藏药全草及根、茎、叶、花等不同部位两种成分的含量.

藏药抱茎獐牙莱HPLC指纹图谱研究

采用反相高效液相色谱-二极管阵列的检测方法,对不同产地的10批野生和栽培抱茎獐牙菜药材的水溶性成分进行了分析,建立了抱茎獐牙菜药材的指纹图谱.色谱柱为VP-ODS C18柱(5 μm,150 mm×4.6 mm),流动相为甲醇-0.02%的磷酸水溶液,检测波长254 nm.用文中的最佳条件可较全面地反映抱茎獐牙菜的主要成分,为藏药抱茎獐牙菜的质量控制提供了科学依据.

HPLC法测定麻黄及其两种制剂中麻黄碱的含量

麻黄为常用中药,其中含有多种有机胺类生物碱,主要成分为L-麻黄碱、D-麻黄碱,具有松弛平滑肌、收缩血管、抗炎、兴奋中枢等作用[1],但如果用量过大或长期使用,会产生震颤、焦虑失眠、心悸等副作用,其含量常作为评价药材品质及其复方制剂质量标准的主要指标[2].麻杏石甘丸和鹏力止鼾颗粒均是以麻黄为主要原料的复方制剂,因此对其进行含量测定是控制麻杏石甘丸和鹏力止鼾颗粒质量的关键.目前国内外学者对麻黄中麻黄碱含量的测定报道较多[3,4],本文采用HPLC法测定其中的麻黄碱含量,现将结果报道如下。

青藏高原红景天药材的HPLC指纹图谱

利用高效液相色谱法建立了青藏高原红景天的色谱指纹图谱.固定相采用C18反相色谱柱,流动相为甲醇:0.1%磷酸水(v/v＝15:85);检测波长220 nm;流速为1.0 mL/min.通过比较发现红景天样品的8个主要共有峰,可作为鉴别红景天药材的主要依据.方法简便快速,为中药品种的鉴定提供了较全面的信息.

高寒藏药--抱茎獐牙菜组织培养研究及其愈伤组织有效成分的测定

从抱茎獐牙菜的胚轴、幼叶及未成熟种子诱导出愈伤组织并再生植株,试验选用MS、B5 和N6 三种培养基,其中以附加2. 4 - D3. 0mg/ L + 6 - BA0. 5mg/ L的MS 培养基诱导率最高;以附加6 - BA0. 5mg/ L + NAA 0. 2mg/ L 的MS 培养基分化苗频率最高;以附加2. 4 - D2. 0mg/ L + 6 - BA0. 5mg/ L 的MS 培养基愈伤组织的生长最好。结果表明,外植体,培养基,激素等对愈伤组织诱导、继代和分化均有明显影响。采用高压液相色谱法(HPLC) 测定抱茎獐牙菜愈伤组织中齐墩果酸含量的结果表明,愈伤组织中齐果墩酸含量因培养基、继代培养时间的不同而有所差异。

LC-DAD-ESI-MS Characterization of Carbohydrates Using a New Labeling Reagent

A novel labeling reagent 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) coupling to liquid chromatography with electrospray ionization mass spectrometry for the detection of carbohydrates from the derivatized rape bee pollen samples is reported. Carbohydrates are derivatized to their bis-NMP-labeled derivatives. Derivatives showed an intense protonated molecular ion at m/z [M+H](+) in positive-ion detection mode. The mass-to-charge ratios of characteristic fragment ions at m/z 473.0 could be used for the accurately qualitative analysis of carbohydrates. This characteristic fragment ion is from the cleavage of C2-C3 bond in carbohydrate chain giving the specific fragment ions at m/z [MH-CmH2m+1Om-H2O](+) for pentose, hexose and glyceraldehydes and at m/z [MH-CmH2m-1Om+1-H2O](+) for alduronic acids such as galacturonic acid and glucuronic acid (m = n - 2, n is carbon number of carbohydrate). No interferences for all aliphatic and aromatic aldehydes presented in natural environmental samples were observed due to the highly specific parent mass-to-charge ratio and the characteristic fragment ions. The method, in conjunction with a gradient elution, offered a baseline resolution of carbohydrate derivatives on a reversed-phase Hypersil ODS-2 column. The carbohydrates such as mannose, galacturonic acid, glucuronic acid, rhamnose, glucose, galactose, xylose, arabinose and fucose can successfully be detected.

Simultaneous determination of monoamine and amino acid neurotransmitters in rat endbrain tissues by pre-column derivatization with high-performance liquid chromatographic fluorescence detection and mass spectrometric identification

A sensitive and efficient method for simultaneous determination of glutamic acid (Glu), gamma-amino-butyric acid (GABA), dopamine (DA), 5-hydroxytryptamine (5-HT) and 5-hydroxyindole acetic acid (5-HIAA) in rat endbrains was developed by high-performance liquid chromatography (HPLC) with fluorescence detection and on-line mass spectrometric identification following derivatization with 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC). Different parameters which influenced derivatization and separation were optimized. The complete separation of five neurotransmitter (NT) derivatives was performed on a reversed-phase Hypersil BDS-C-18 column with a gradient elution. The rapid structure identification of five neurotransmitter derivatives was carried out by on-line mass spectrometry with electrospray ionization (ESI) source in positive ion mode, and the BCEOC-labeled derivatives were characterized by easy-to-interpret mass spectra. Stability of derivatives, repeatability, precision and accuracy were evaluated and the results were excellent for efficient HPLC analysis. The quantitative linear range of five neurotransmitters were 2.441-2 x 10(4) nM, and limits of detection were in the range of 0.398-1.258 nM (S/N = 3:1). The changes of their concentrations in endbrains of three rat groups were also studied using this HPLC fluorescence detection method. The results indicated that exhausting exercise could obviously influence the concentrations of neurotransmitters in rat endbrains. The established method exhibited excellent validity, high sensitivity and convenience, and provided a new technique for simultaneous analysis of monoamine and amino acid neurotransmitters in rat brain. (C) 2008 Elsevier B.V. All rights reserved.

Separation and determination of the major active components in Tibetan folk medicinal species Swertia franchetiana by HPLC with DAD

A sensitive and specific reversed-phase high performance liquid chromatography (RP-HPLC) method with diode array detection (DAD) was established for the quantitative determination of the nine active components, namely, swertiamarin (SWM, 1), mangiferin (MA, 2), gentipicroside (GE, 3), sweroside (SWO, 4), isoorientin (IS, 5), swertisin (SWS, 6), swertianolin (SWN, 7), 7-O-[alpha-L-rhamnopyranosyl-1 -> 2)-beta-D-xylopyranosyl]-1,8-dihydroxy-3-methoxyxanthone (RX, 8), and bellidifolin (BE, 9) used as the external standard, in Tibetan folk medicinal species Swertia franchetiana. Based on the baseline chromatographic separation of most components from the methanolic extract of Swertia franchetiana on a reversed-phase Eclipse XDB-C8 column with water-acetonitrile-formic acid as mobile phase, the nine components were identified by comparison with standard samples and qualified by using the external standard method with DAD at 254 nm. The correlation coefficients of all the calibration curves were found to be higher than 0.9980. The relative standard deviations (RSDs) of the peak areas and retention times for the nine standards were less than 2.07% and 2.86%, respectively.