共查询到19条相似文献,搜索用时 46 毫秒
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高速逆流色谱法分离纯化黄芪中的芒柄花素和毛蕊异黄酮 总被引:19,自引:0,他引:19
采用高速逆流色谱法(HSCCC),以正己烷-氯仿-甲醇-水组成二相系统作为固定相与流动相,对黄芪的乙酸乙酯粗提
物进行了分离纯化。 结果发现:以正己烷-氯仿-甲醇-水(体积比为1.5∶3∶3∶2)组成的系统可以从黄芪的乙酸乙酯粗
提物中分离出毛蕊异黄酮,纯度可达95%以上,并可以初步纯化芒柄花素;接着用正己烷-氯仿-甲醇-水(体积比为4∶4∶5
∶4)组成的系统进一步纯化芒柄花素,其纯度达95%以上。利用该方法,可以对中药黄芪中的异黄酮进行快速的分离和纯
化。 相似文献
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建立了超高效液相色谱-电喷雾串联三重四级杆质谱法(UPLC-ESI-MS)同时测定贞芪扶正胶囊中红景天苷、毛蕊异黄酮-7-O-β-D-葡萄糖苷和黄芪甲苷含量的方法.采用UPLC-ESI-MS联用法,乙腈和0.3%甲酸水溶液不同比例梯度洗脱,流速0.3 m L/min,12 min内可完成测试,且线性关系良好(r20.999).方法简便、准确、可靠、重复性好,可用于贞芪扶正制剂的质量控制. 相似文献
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高效液相色谱-蒸发光散射检测法测定玉屏风胶囊中黄芪甲苷的含量 总被引:4,自引:0,他引:4
建立高效液相色谱-蒸发光散射检测法测定玉屏风胶囊中黄芪甲苷的含量.采用Phenomenex C18(4. 6mm×250 mm i. d. ,5μm)色谱柱,柱温为35℃,以乙腈-水(35∶65)为流动相,以蒸发光散射检测器进行检测.以峰面积的常用对数(Y)对进样量的常用对数(X)进行线性回归,回归方程为Y=1. 6709 X+14. 2699(r=0. 9998),线性范围为1~19μg.加标回收率为86. 7%~96. 2%,测定结果的RSD为0. 22%(n=7).方法准确、可靠、重复性好,可有效控制玉屏风胶囊的质量. 相似文献
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用HPLC测定虫草酒中的黄芪甲甙 总被引:1,自引:0,他引:1
为了控制虫草酒质量,采用高效液相色谱(HPLC)法以YWG-G18为固定相,乙腈-水(1:2)+0.15%磷酸为流动相,UV检测,波长为205nm。测定了虫草酒中黄芪甲甙的含量,方法简便,结果准确,回收率分别为92.37%~97.27%。RSD为1.47%,能满足质量标准控制要求。 相似文献
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膜荚黄芪与蒙古黄芪化学成分的高效液相色谱-质谱研究 总被引:5,自引:0,他引:5
采用高效液相色谱-质谱联用技术对膜荚黄芪及蒙古黄芪药材的甲醇提取物进行了对比分析。选用Inertsil ODS C18不锈钢柱,以乙腈-水梯度洗脱,流速1.0mL/min,柱温25℃,二级管阵列(PDA)和电喷雾电离质谱(ESI-MS)同时在线检测。通过与标准品对照、紫外光谱及多级质谱分析并与文献对照鉴定了14个成分,分别是:毛蕊异黄酮-7-O-β-D-吡喃葡萄糖苷(1)、芒柄花苷(2)、9,10.二甲氧基紫檀烷.3-O-β-D.吡喃葡萄糖苷(3)、2’-羟基-3’,4’-二甲氧基异黄烷-7-O-β-D-吡喃葡萄糖苷(4)、毛蕊异黄酮(5)、黄芪甲苷(6)、黄芪皂苷Ⅱ(7)、异黄芪皂苷Ⅱ(8)、芒柄花素(9)、黄芪皂苷Ⅰ(10)、异黄芪皂苷Ⅰ(11)、蔗糖(12)、毛蕊异黄酮(7-O-β-D-吡喃葡萄糖苷-6″-O-丙二酸酯(13)、乙酰黄芪皂苷Ⅰ(14)。经对比发现,膜荚黄芪和蒙古黄芪的主要化学成分相似但也存在一些差异。对黄芪主要成分的电喷雾质谱裂解规律进行了归纳总结。 相似文献
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高效液相色谱法测定葡萄叶中5种芪化物 总被引:3,自引:0,他引:3
建立了同时检测葡萄叶片中白藜芦醇(resveratrol,Res)、云杉苷(piceide,PD)、ε-葡萄素(ε-viniferin)、δ-葡萄素(δ-viniferin)、紫檀芪(pterostilbene,PS)5种芪化物的高效液相色谱分析方法.采用Atlantis C18色谱柱 (250 mm×4.6 mm, 5 μm), 流动相为乙腈、水梯度洗脱,二极管阵列检测器,检测波长为306 nm;流速1 mL/min; 柱温30 ℃,外标法定量.结果显示: 5种芪化物的线性关系良好,相关系数在0.9990~0.9996之间;精密度、稳定性的RSD都低于5%;平均回收率为90.3%~114.0%,检出限为0.01~0.05 mg/L.本方法前处理简单、快速.应用本方法测定了葡萄叶片紫外诱导后5种芪化物的含量变化,结果令人满意. 相似文献
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高效液相色谱-电喷雾质谱法测定红车轴草中异黄酮类化合物 总被引:6,自引:0,他引:6
采用高效液相色谱与电喷雾质谱联用技术研究了红车轴草中的异黄酮类化合物。实验采用反相C18色谱柱,二元线性梯度洗脱,分离并检测了红车轴草中的14种异黄酮类化合物;通过与电喷雾质谱联用获得了相应化合物的分子量信息,并利用质谱的源内碰撞诱导解离技术鉴定这些化合物的可能结构分别为:大豆苷、野靛苷-7-O-β-D-葡萄糖苷、芒柄花苷、德鸢尾素-4'-O-β-D-葡萄糖苷、大豆苷元、印度黄檀苷、樱黄素-4'-O-β-D-葡萄糖苷、染料木素、红车轴草素、芒柄花素、樱黄素、鹰嘴豆芽素A、野靛苷和德鸢尾素。 相似文献
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考察了超临界流体色谱(SFC)中的色谱柱、改性剂、添加剂、流速、柱温和背压等因素对9种黄酮类成分(包括芒柄花素、异鼠李素、毛蕊异黄酮、山奈酚、槲皮素、紫云英苷、芒柄花苷、异槲皮苷、毛蕊异黄酮葡萄糖苷)分离的影响,与高效液相色谱法(HPLC)进行了比较,并建立了黄芪饮片中5种主要黄酮类化合物的SFC分析方法。采用Agilent ZORBAX RX-SIL色谱柱(4.6 mm × 150 mm,5 μm)进行分离,CO2-0.1%磷酸甲醇溶液为流动相梯度洗脱,流速为3 mL/min;柱温为35 ℃;背压为10 MPa,9种黄酮类化合物可在10 min内实现基线分离。5种黄酮类化合物在一定质量浓度范围内均具有良好的线性关系(r2 ≥ 0.963 2),检出限为10.69 ~ 16.21 μg/mL,日内相对标准偏差(RSD)为1.3% ~ 2.0%;日间RSD为1.6% ~ 2.2%。5种黄酮类化合物在48 h内具有良好的稳定性,重复性为3.6% ~ 6.0%,回收率为91.8% ~ 112%。与HPLC法相比,9种化合物的保留时间顺序基本相反,SFC法更快速、经济环保,且其保留及选择性受色谱柱、改性剂和添加剂的影响较大,添加剂对色谱峰形影响明显。 相似文献
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YUE Gui-Hua YANG Peng-Yuan SHEN Xian-Rong JI Dong-Mei REN Da-Ming XU Yun-Ming LIU Wei-Ping WANG Hong-Hai 《高等学校化学学报》1999,20(Z1):468
The bio-mass spectrometry has been become an important analytical tool in Life Science such as in searching for a functional protein in disease treatments, for example, the proteins with a function of antiangiogenesis. If an unknown functional protein can be identified and characterized, it is then possible to mass-produce this protein through bio-techniques and the technique of genetic engineering. 相似文献
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Photolysis of imazosulfuron was studied in aqueous solution under UV light. The reaction followed a pseudo-first-order kinetic with significant correlation coefficient. The major photodegradation products of imazosulfuron after irradiation under UV light were separated and tentatively identified by HPLC-MS analysis as (4,6-dimethoxypyrimidine-2-yl)aminocarbonylsulfamic acid, 4,6-dimethoxy-2-ureidopyrimidine and 2,2'-dichloro-[3,3'] bi [imidazo[1,2-a] pyridinyl]. The results indicate that different reaction pathways are followed: (1) cleavage of the sulfonylurea bridge; (2) desulfonylation, which can proceed either by a carbon-sulfur cleavage or a nitrogen-sulfur cleavage. A mechanism for the formation of the photoproducts is proposed. 相似文献
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鲨鱼软骨血管抑制因子的高效液相色谱与电喷雾质谱研究 总被引:3,自引:0,他引:3
电喷雾质谱 ( ESIMS)具有快速、灵敏等特点 ,近年来已成为鉴定和分析多肽、蛋白质和核酸的有力工具 .将 ESIMS与高效液相色谱 ( HPLC)联用 ,在蛋白质分子量、结构及活性位点等方面的研究已取得较大的进展 [1 ] .鲨鱼软骨血管抑制因子 ( SCAIF- I)是作者之一从鲨鱼软骨中提取的一种未知蛋白质[2 ] ,研究表明 ,SCAIF- I对肿瘤、癌症的抑制及治疗具有明显的疗效[3] .因此 ,对其结构的研究具有重要的意义 .本文报道了用 HPL C与 ESIMS对未知蛋白质 SCAIF- I的分子量及肽段部分序列的测定结果 .1 实验部分1 .1 样品制备 SC… 相似文献
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《液相色谱法及相关技术杂志》2012,35(17):3455-3463
Abstract Oxime derivatives of a number of steroidal 4-en-3-one 17-alcohols and 17-esters have been separated into syn and anti isomers by HPLC under normal or reverse-phase conditions. The elution order of the isomeric pairs was found to vary with the nature of the steroid and the type of stationary phase: a peak ratio method at two wavelengths provides a very convenient method for unambiguously identifying the geometries of the isomeric pairs. 相似文献
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Hassan Madkhali Amer Tarawneh Zulfiqar Ali Hoang V. Le Stephen J. Cutler Ikhlas A. Khan Zia Shariat-Madar 《Molecules (Basel, Switzerland)》2021,26(14)
The goal of this study was to assess the pharmacological effects of black tea (Camellia sinensis var. assamica) water extract on human kinin-forming enzymes in vitro. Tea is a highly consumed beverage in the world. Factor XII (FXII, Hageman factor)-independent- and -dependent activation of prekallikrein to kallikrein leads to the liberation of bradykinin (BK) from high-molecular-weight kininogen (HK). The excessive BK production causes vascular endothelial and nonvascular smooth muscle cell permeability, leading to angioedema. The prevalence of angiotensin-converting enzyme inhibitor (ACEI)-induced angioedema appears to be through BK. Both histamine and BK are potent inflammatory mediators. However, the treatments for histamine-mediated angioedema are unsuitable for BK-mediated angioedema. We hypothesized that long-term consumption of tea would reduce bradykinin-dependent processes within the systemic and pulmonary vasculature, independent of the anti-inflammatory actions of polyphenols. A purified fraction of the black tea water extract inhibited both kallikrein and activated FXII. The black tea water extracts inhibited factor XII-induced cell migration and inhibited the production of kallikrein on the endothelial cell line. We compared the inhibitory effects of the black tea water extract and twenty-three well-known anti-inflammatory medicinal herbs, in inhibiting both kallikrein and FXII. Surprisingly, arjunglucoside II specifically inhibited the activated factor XII (FXIIa), but not the kallikrein and the activated factor XI. Taken together, the black tea water extract exerts its anti-inflammatory effects, in part, by inhibiting kallikrein and activated FXII, which are part of the plasma kallikrein–kinin system (KKS), and by decreasing BK production. The inhibition of kallikrein and activated FXII represents a unique polyphenol-independent anti-inflammatory mechanism of action for the black tea. 相似文献
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ShiLanFENG FangDiHU JianXiongZHAO JingWenXU LiRenCHEN 《中国化学快报》2004,15(11):1335-1338
Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 commonpeaks were analyzed, their average similarity was 97.29%. CFP were positioned with main indexcomposition such as formononetin, calycosin and then the contents of index composition weredetermined. The character and exclusive of CFP of 10 samples of hongqi were clear. CFP andcontent determination of index composition of hongqi could be used to evaluate the quality of hongqicomprehensively. 相似文献
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《Analytical letters》2012,45(12):2253-2262
Abstract A Reverse-Phase HPLC method is described for the simultaneous identification and determination of 5 barbiturates: Allobarbital, Phencbarbital, Butabarbi -tal, Butalbital and Pentobarbital. Barbital is used as internal standard. The mobile phase is Milli Q Water/ Acetonitrile/ 1.75 M Phosphoric Acid (738:200:2, v/v/v) at a flow rate of 0.8 mL/min and UV detection is carried out at 195 nm. The single extraction procedure requires only small samples and analysis is quick. 相似文献
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A high-performance liquid chromatography (HPLC) unit equipped with size exclusion column and a refractive index detector was
used for simultaneous monitoring, identification, and quantitation of the reaction components from lipase-catalyzed transesterification
of three oils. The procedure simultaneously separated and detected the unreacted triacylglycerols (TAG), diacyl-, and monoacyl-glycerol
(DAG and MAG) co-products, residual alcohol as well as free fatty acid (FFA) based on retention times. The chromatograms showed
well separated and resolved peaks. The elution of the components from the transesterification reaction in increasing order
was: TAG < DAG < FFA < MAG. Generally, higher alcohol ratios decreased the conversion of TAG in all the oils studied with
between 14% and 94% of TAG remaining at all the treatment combinations. Higher amount of salmon skin oil (SSO) TAG was generally
converted to DAG than Rothsay composite (RC) and olive oil (OO) TAG. Relatively higher amount of OO DAG was converted to MAG
than SSO and RC with only 5–14% DAG remaining in OO. RC and OO generally accumulated less MAG, and this was reflected as lower
MAG levels in RC (<6%) and OO (<14%) compared with SSO (<27%). For the various treatment combinations and the three oils used
in this study, the least amount of FFA was recorded in transesterified OO with a maximum of approximately 4%. This HPLC method
can be used as a simple and fast technique to analyze the reaction components and products of transesterification reactions
without the need for additional derivatization steps. 相似文献