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1.
高效液相色谱法测定糖脂双降茶中淫羊藿甙的含量 总被引:4,自引:0,他引:4
建立了高效液相色谱法测定糖脂双降茶中淫羊藿甙含量的方法。采用ODS柱 ,以甲醇 水 (体积比为 60∶4 0 )为流动相 ,用紫外检测器于 2 70nm处检测。结果表明 ,淫羊藿甙的质量浓度在 0 1g/L~ 0 5 g/L范围内与色谱峰的峰面积呈良好的线性关系 (r =0 9993 ) ,回收率为 10 1 0 %~ 10 1 7% ,RSD为 1 6%~ 2 7% (n =3 )。方法快速、简便、准确 ,结果稳定 ,重现性好 ,可推荐其作为质量检验的一个定量方法。 相似文献
2.
HPLC法同时测定淫羊藿中朝藿定A、B、C与淫羊藿苷的含量 总被引:8,自引:0,他引:8
建立了同时测定淫羊藿中朝藿定A、B、C与淫羊藿苷含量的高效液相色谱方法。淫羊藿样品经超声波提取,以50%(φ)乙醇溶液为溶剂,在温度50℃、料液比1∶60条件下超声波提取30 m in,共提取2次。色谱条件:ZORBAX SB-C8色谱柱(5μm,4.6×250 mm);流动相A为乙腈,B为1%乙酸溶液;梯度洗脱;紫外检测波长为270 nm。上述4种类黄酮的标准曲线在6.6~33.0 mg/L(朝藿定A、淫羊藿苷)或6.6~55.0mg/L(朝藿定B、C)范围内呈良好的线性关系(r>0.99);加标回收率在97%~102%之间;相对标准偏差小于2%(n=5)。测得不同产地心叶淫羊藿叶片中4种类黄酮的质量分数差异较大;朝藿定A广泛分布于淫羊藿属中。本方法在淫羊藿药材质量控制中具有一定的参考价值。 相似文献
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淫羊藿甙和朝藿定A、B、C是淫羊藿中重要的活性成分,本研究应用工业制备高效液相色谱从淫羊藿粗提物中分离制备了这4个成分。淫羊藿粗提物经大孔吸附树脂粗分离获得相应的组分后,利用工业制备高效液相色谱完成精制纯化。采用自装填Chromatorex C18制备柱(220 mm×77 mm, 10 μm),乙腈-水(26:74或30:70, v/v)为流动相进行洗脱,在35 min内,实现了这4种成分的基线分离及规模制备。从300 g粗提物(总黄酮含量约20%)中获得淫羊藿甙33 g、朝藿定C 4.6 g、朝藿定B 3.7 g和朝藿定A 0.6 g,产品纯度均达到98%以上。此方法通过两步分离即可实现这4种成分的完全分离,具有快速高效、产品纯度高的特点,适于淫羊藿中淫羊藿甙、朝藿定A、B、C系列对照品的规模制备。 相似文献
4.
固体表面室温烯光法测定淫羊藿甙 总被引:1,自引:0,他引:1
1引言 淫羊藿甙(cariin)为中草药淫羊藿的主要有效成分,有增加冠脉血流量的作用.淫羊甙的测定方法有薄层扫描法,高效液相色谱法等.固体表面室温燐光法是一种微量技术与痕量分析相结合的分析方法,而淫羊藿甙的室温燐光法的研究未见文献报道.本文以cd(c)2为重原子微扰剂,以聚酰胺膜作基质时,能诱导出淫羊藿甙的RTP发射.其激发波长为300nm(弱峰)和400nm(强峰),发射波长为500nm.淫羊藿甙含量在1.35~675ng/斑范围内与RTP强度呈良好的线性关系,检出限达0.06ng/斑.该法具有操作简便,灵敏度高,线性范围宽,取样量少的特点. 相似文献
5.
离子对色谱法测定万乳康注射液中淫羊藿苷和盐酸左旋咪唑含量 总被引:1,自引:0,他引:1
建立了反相离子对色谱法同时测定万乳康样品中淫羊藿苷和盐酸左旋咪唑的含量。本法使用Shim-pack VP-ODS色谱柱(250×4.6 mm,5μm),该流动相为65%甲醇(V/V),10.0 mmol/L的十二烷基磺酸钠,pH=3.0;等度洗脱样品中的淫羊藿苷和盐酸左旋咪唑。紫外检测波长270 nm。结果表明:淫羊藿苷测定的线性范围为2.73~54.58μg/mL,加标回收率为99.45%~100.69%,理论塔板数达6 641;盐酸左旋咪唑测定的线性范围为26.23~524.54μg/mL,加标回收率为99.58%~100.23%,理论塔板数5 564。该方法可用于淫羊藿提取物和万乳康样品中的淫羊藿苷和盐酸左旋咪唑的测定。 相似文献
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朝鲜淫羊藿中一种黄酮醇甙的化学结构 总被引:2,自引:0,他引:2
朝鲜淫羊藿中一种黄酮醇甙的化学结构李文魁,肖培根,廖矛川,张如意(中国协和医科大学药用植物研究所,北京,100094)(北京医科大学药学院)关键词朝鲜淫羊藿,黄酮醇甙,结构分析前文[1]中我们报道了从朝鲜淫羊藿(EpimediumkoreanumNa... 相似文献
9.
建立了固相萃取(SPE)/定量核磁共振波谱(q NMR)无标样测定乳增宁胶囊中有效成分淫羊藿苷含量的方法。样品用10%乙醇室温下超声提取,以HC-C18型SPE柱对提取液进行浓缩除杂后,用q NMR测定淫羊藿苷的含量。考察了超声时间、SPE样品前处理条件以及定量核磁共振实验条件对定量结果的影响。选择氘代二甲基亚砜为溶剂,2,3,5-三碘苯甲酸为内标,并用基准试剂邻苯二甲酸氢钾对其进行标定。选择脉冲宽度P1=14.1μs,扫描次数NS=256为q NMR定量淫羊藿苷的实验条件。淫羊藿苷的定量峰为δ7.9(2',6'-H,d,2H)。结果显示,所建方法的日内精密度RSD为0.43%,日间精密度RSD为0.75%,淫羊藿苷与2,3,5-三碘苯甲酸峰面积比与质量比的零截距标准曲线的线性相关系数为0.999 9,且斜率与理论值相符。该法测定淫羊藿苷的LOD为0.122 mg/g;LOQ为0.368 mg/g。样品经SPE预处理后淫羊藿苷的回收率为99.8%~103.0%。可在不用对照品的情况下对乳增宁胶囊中淫羊藿苷的含量进行测定。 相似文献
10.
固体表面室温燐光法测定淫羊藿甙 总被引:1,自引:0,他引:1
1引言 淫羊蕾甙(icariin)为中草药淫羊蕾的主要有效成分,有增加冠脉血流量的作用。淫羊蕾甙的测定方法有薄层扫描法,高效液相色谱法等。固体表面室温光法是一种微量技术与痕量分析相结合的分析方法,而建羊蕾甙的室温光法的研究未见文献报道。本文以Dd(Ac)2为重原子微扰剂,以聚酰胺膜作基质时,能诱导出淫羊藿甙的RTP发射。其激发波长为300nm(弱峰)和400nm(强峰),发射波长为500nm。淫羊藿甙含量在1.35~675 ng/斑范围内与RTP强度呈良好的线性关系,检出限达0,06 ng/斑。该… 相似文献
11.
In this paper, the dissociation constants (pKa1, pKa2) of five anthraquinones were determined from the relation between the effective mobility at different pH values and the buffer pH value, which was derived from the basic electrophoresis theory and the dissociation equilibrium of a binary acid. In addition, the changes of pKa values of the five compounds were also investigated when organic modifiers were added to the buffer system. 相似文献
12.
Herba Epimedii (family Berberidaceae), Ying-Yang-Huo in Chinese, is a famous Chinese herbal medicine. Flavonoids are thought to be the major active components in it. A capillary zone electrophoresis (CZE) separation were developed for simultaneous determination of four flavonoids including icariin, epimedin A, epimedin B and epimedin C in Epimedium. The effects of the experimental variables on CZE had been optimized by using central composite design (CCD). The best separation of four flavonoids could be obtained using 50 mM borate buffer (pH 10.0) containing 22% acetontrile as modifier, while separation voltage was 15 kV and temperature was at 25 degrees C. The method developed is accurate, simple and reproducible, which could be used for quality control of Epimedium and its medical preparations. 相似文献
13.
淫羊藿属药材反相高效液相色谱指纹图谱及质量评估研究 总被引:6,自引:0,他引:6
用一种新的多台阶梯度洗脱的反相高效液相色谱(RPLC)法, 首次建立了秦岭山区产4种产地及亚属均不相同的淫羊藿属药材的由9种成分组成的色谱指纹图谱. 并以淫羊藿甙为内标作为相对标准, 对其质量进行了评估. 然而, 因其产地和亚属的不同, 指纹图谱又各有特征, 发现产地不同的两种淫羊藿亚属, 箭叶淫羊藿的RPLC指纹图谱由12个色谱峰组成. 还提出用相对含量比较法对各种类淫羊藿中9种成分的含量进行了质量评价. 本工作所建立的淫羊藿属药材的RPLC指纹图谱法从试样提取的精密度、稳定性、图谱重复性等方面均符合《中药注射剂指纹图谱研究的技术要求(暂行)》中的有关规定. 该方法具有重现性好, 特征性强, 方法简便、快速等特点, 有可能成为淫羊藿药材种属判断、质量评估的标准, 也会对未来开发淫羊藿中其他有效成分提供科学的依据. 相似文献
14.
Herba Epimedii (known as Yinyanghuo in China) is one of the commonly used Chinese medicines. Flavonoids are considered as its active components. In this study, a CEC method was developed for the simultaneous determination of seven flavonoids, including hexandraside E, kaempferol-3-O-rhamnoside, hexandraside F, icariin, epimedin A, B, and C, in Epimedium using baicalein as internal standard (IS). The influence of relevant parameters such as buffer concentration, pH, and proportion of ACN was investigated and optimized. Baseline separation was obtained using a Hypersil C18 capillary (3 microm, 100 microm/25 cm) with a mixture of 20 mM phosphate buffer (pH 4.0)/ACN (70:30 v/v) as mobile phase running at 30 kV and 25 degrees C in 20 min. All calibration curves showed good linearity (r2 >0.9992) within test ranges. The LOD and LOQ were lower than 8.6 and 42.8 microg/mL, respectively. The RSDs of intra- and interday for relative peak areas of seven analytes were less than 3.1 and 4.4%, and the recoveries were 95.2-103.3%. Samples of different Epimedium species were analyzed using the validated method, which is useful for quality control of Epimedium and its medical preparations. 相似文献
15.
毛细管区带电泳测定芦荟中的有效成分 总被引:11,自引:0,他引:11
建立了毛细管区带电泳测定中药芦荟中的有效成分芦荟甙和芦荟大黄素的分析方法。采用24 mmol/L的磷酸盐(pH 10.85)作为缓冲溶液,在电压为15 kV和检测波长为254 nm的条件下进行分离实验,芦荟提取液中有效成分获得基线分离。定量分析表明,芦荟甙的质量浓度为0.029 g/L~1.00 g/L时,其峰面积与质量浓度呈线性关系(r=0.997);芦荟大黄素的质量浓度为5.4 mg/L~84 mg/L时,其峰面积与质量浓度呈线性关系(r=0.999)。此外,还讨论了缓冲溶液的pH值、有机改性剂对两种有效成分迁移行为的影响。 相似文献
16.
Electrophoretic behavior study and determination of some active components in Chinese medicinal preparations by capillary electrophoresis 总被引:4,自引:0,他引:4
The determination of icariin (IC), rhein (RH), chrysophanol (CH), physcion (PHY), glycyrrhetic acid (GE), and glycyrrhizic acid (GI), in traditional Chinese preparations, Anshen Bunao oral liquid and Maren pill, has been investigated by micellar electrokinetic capillary electrophoresis. With borate buffer (10 mM), SDS (20 mM) and acetonitrile (10%) as background electrolyte (pH 9.55), 20 kV applied voltage and 254 nm UV detection, the six active compounds were completely separated within 10 min. The effects of buffer pH, concentration of borate, SDS and modifier on electrophoretic behavior and separation are discussed. Regression equations revealed linear relationships (correlation coefficients: 0.9960-0.9999) between the peak-area of each component and the content. In addition, the levels of the six active compounds in two kinds of traditional Chinese medicinal preparations were easily determined with recoveries of from 94.7% to 106.4%. 相似文献
17.
A preparative high-speed counter-current chromatography (HSCCC) method for isolation and purification of flavonoids from the Chinese medicinal plant Epimedium koreamum Nakai was successfully established by using chloroform-methanol-water (4:3.5:2, v/v) as the two-phase solvent system. The method yielded 11.4 mg of epimedokoreanoside I, 46.5 mg of icariin and 17.7 mg of icariside II from 200 mg of the crude sample in one-step separation with the purity of 98.2%, 99.7% and 98.5%, respectively, as determined by high-performance liquid chromatography (HPLC). The structures of the flavonoids were identified by 1H NMR and 13C NMR. 相似文献
18.
A CE method for investigating the chemico-physical characteristics of the active components of low molecular weight in Gastrodia elata Bl. is described. First, the dissociation constants of five active components were determined based on the relation between the effective mobility of the solutes and the buffer pH value. Second, an equation that describes the relation of the migration time and the molecular weight was developed and used to predict the migration order and to calculate the electroosmotic velocity. The results predicted by theory agreed well with that from experiments. 相似文献
19.
Simultaneous determination of 15 flavonoids in Epimedium using pressurized liquid extraction and high-performance liquid chromatography 总被引:4,自引:0,他引:4
Herba Epimedii (family Berberidaceae), Yinyanghuo in Chinese, is one of the commonly used Chinese medicines. Flavonoids are considered as its active components. In this study, a reliable pressurized liquid extraction (PLE) and HPLC method was developed for simultaneous determination of 15 flavonoids, namely hexandraside E, kaempferol-3-O-rhamnoside, hexandraside F, epimedin A, epimedin B, epimedin C, icariin, epimedoside C, baohuoside II, caohuoside C, baohuoside VII, sagittatoside A, sagittatoside B, 2'-O-rhamnosyl icariside II and baohuoside I in different species of Epimedium. The analysis was performed by using a Zorbax SB-C18 analytical column (250 mm x 4.6 mm I.D., 5 microm) at gradient elution of water and acetonitrile with diode-array detection (270 nm). All calibration curves showed good linearity (r(2)>0.9997) within test ranges. The LOD and LOQ were lower than 1.31 ng and 2.62 ng on column, respectively. The RSD for intra- and inter-day of 15 analytes was less than 3.8% at three levels, and the recoveries were 90.5-106.8%. The validated method was successfully applied for the analysis of 15 flavonoids in different species of Epimedium which had great variation on the contents of investigated flavonoids. Hierarchical clustering analysis based on the characteristics of 15 investigated compound peaks in HPLC profiles showed that 26 samples were divided into three main clusters, which were in accordance with their flavonoid contents. Four flavonoids including epimedin A, B, C and icariin were optimized as markers for quality control of the species of Epimedium used as Yinyanghuo. 相似文献
20.
Characterization of cephalosporin transfer between aqueous and colloidal phases by micellar electrokinetic chromatography 总被引:1,自引:0,他引:1
A new electrokinetic chromatographic method was applied to the determination of the partition coefficient between water and micelle for a group of cephalosporins (cefmetazol, cephradin, cefaclor, ceftazidim, cefodizim, cephapirin, cephalothin and ceftriaxon) using sodium dodecyl sulphate as an anionic surfactant in microemulsion and in micellar systems. In the new method, the running buffer contains both the micelles and the drug, and the injected solution contains the same concentration of micelles as the running buffer but not the drug. The mobility of the drug can be measured from a negative peak recorded the chromatogram. The required parameters for the determination of the capacity factor (mu(aq) and /mu(me) are the electrophoretic mobilities of the solutes in the aqueous and the micelle phases, mu(eff) is the effective mobility in the micellar system or in the microemulsion) were measured by the new micellar and microemulsion electrokinetic chromatography technique. Linear log-log relationships were found between both the micelle-water partition coefficient and the capacity factor and the n-octanol-water partition coefficient. 相似文献