共查询到20条相似文献,搜索用时 93 毫秒
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在0.02 mol/L NH4Cl-NH3.H2O(pH8.0)的底液中,采用循环伏安法测定葛根素,得到一良好的氧化峰,峰电位Ep=+0.57V,峰电流Ip与葛根素的浓度在1.046×10-7~5.767×10-5mol/L范围内成线性关系,相关系数r为0.9989,检出限为1.046×10-7mol/L.测定葛根中葛根素的含量,平均回收率在99.8%.并且研究了葛根素在玻碳电极上的电化学行为,结果表明葛根素的电极过程具有吸附性和不可逆性. 相似文献
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葛根素在酸碱溶液中的紫外光谱特性及应用 总被引:1,自引:0,他引:1
葛根素在酸碱溶液中具有不同的紫外吸收光谱特性。以葛根素碱溶液为测定液,以等浓度的葛根素水溶液为参比液,用差示法测定其吸光度。结果表明:在337 nm处,当葛根素浓度为1.0×10-5~1.0×10-4mol/L时,吸光度与浓度之间存在良好的线性关系,据此建立了测定葛根素的差示紫外光谱法。用此法直接测定了葛根和葛根素注射液中葛根素的含量,平均回收率分别为99.5%(RSD=1.66%)、99.7%(RSD=0.85%)。本法结果与高效液相色谱(HPLC)法对照,对同一样品进行对照测定,结果令人满意。 相似文献
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建立了一种新的胶束毛细管电泳方法,用于同时分离检测葛根素、大豆苷、 3’-甲氧基葛根素、 3’-羟基葛根素和4’-甲氧基葛根素5种异黄酮。优化的实验条件为:以40 mmol/LNa2B4O7+4 mmol/L NaOH(pH 9.62)为运行缓冲溶液,5%(V/V)甲醇和14 mmol/L的十二烷基磺酸钠(SDS)为添加剂,分离电压22 kV,检测波长250 nm,进样时间5 s。在优化条件下,葛根素、大豆苷、 3’-甲氧基葛根素、 3’-羟基葛根素和4’-甲氧基葛根素5种异黄酮可在14 min内完成分离检测,各目标组分的峰面积与其浓度之间的线性关系良好。该方法用于葛根及其制剂中5种异黄酮的定量分析,加标回收率范围为95.6%~104.8%,相对标准偏差不超过4.0%。 相似文献
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建立高效液相色谱测定葛根芩连片中葛根素含量的方法。以体积分数50%的甲醇为提取液对样品超声提取20 min,采用DiamonsilTMC18(250 mm×4.6 mm,5μm)色谱柱,以甲醇–乙腈–水(体积比8∶12∶80)为流动相,流速为1.0 mL/min,检测波长为250 nm,柱温为30.0℃,进样量体积10μL。在最佳实验条件下,葛根素与其它物质能完全分离,葛根素的质量浓度在5.43~543.2μg/mL范围内与色谱峰面积呈良好的线性,线性相关系数r=0.999 9,方法检出限为3.50μg/mL(S/N=3)。方法加标回收率为100.0%,测定结果的相对标准偏差为1.6%(n=6)。该方法简单、快速、重现性好,适用于葛根芩连片中葛根素的测定。 相似文献
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采用静态吸附法考察了D101、AB-8、NKA-2、NKA-9、HPD 100、HPD600等6种大孔吸附树脂对(R,S)-告依春的吸附及解吸性能,筛选出效果最佳的AB-8树脂,并对其进行动态考察.最佳富集条件为:上样液pH 6,生药质量-体积浓度为0.200g/mL,解吸液为2BV量70%乙醇,在优化条件下(R,S)-告依春在浸膏中含量可从0.76%提高到12.48%.结果表明,AB-8型大孔吸附树脂可用来从板蓝根水提取液中富集(R,S)-告依春. 相似文献
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Regarding hydrophilic interaction chromatography and normal phase liquid chromatography, RPLC is another choice used to separate polar compounds with the improvement of polar-modified C18 stationary phase. In this study, a method using conventional C18 column coupled with polar-copolymerized C18 column was successfully developed for the separation and purification of polar compounds from Radix isatidis, which is one of the most commonly used traditional Chinese medicines (TCMs). An XTerra MS C18 column was used to fractionate the extract of R. isatidis and a homemade polar-copolymerized C18 column was utilized for the final purification due to its good separation selectivity and high resolution for polar compounds. The established purification system demonstrated good orthogonality for the polar compounds. As a result, ten compounds were purified and three of them were identified as 3-methyl-5-vinyloxazolidin-2-one (compound A), 5-hydroxymethyl-2-furaldehyde (compound B) and 3-methylfuran-2-carboxylic acid (compound G) based on the MS, IR and extensive NMR data, respectively. It was demonstrated to be a feasible and powerful technique for the purification of polar compounds under RPLC mode and more chemical information of TCMs will be obtained to interpret the efficiency of TCMs. 相似文献
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高效液相色谱-质谱分析指导下制备黄芩中系列黄酮成分对照品 总被引:1,自引:0,他引:1
在高效液相色谱-质谱分析指导下,针对性地分离制备了黄芩药材中系列黄酮成分对照品。首先对黄芩药材乙醇提取物进行液相色谱-质谱分析,获得各色谱峰的保留时间、紫外光谱和质谱特征。经波谱数据解析结合文献对比,鉴定了黄芩药材中的19种黄酮类成分。然后根据液相色谱-质谱分析结果和文献,设计了目标成分对照品的制备流程,采用低压制备柱色谱法依次制备了黄芩苷、汉黄芩苷、黄芩素、汉黄芩素和千层纸素A共5种黄酮类成分的对照品。结果表明这5种黄酮类成分对照品的纯度均大于98%。该方法可用于针对性地快速分离制备中药中的化学成分。 相似文献
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Chen SB Liu HP Tian RT Yang DJ Chen SL Xu HX Chan AS Xie PS 《Journal of chromatography. A》2006,1121(1):114-119
The roots of Pueraria lobata (Wild.) Ohwi and Pueraria thomsonii Benth have been officially recorded in all editions of Chinese Pharmacopoeia under the same monograph 'Gegen' (Radix Puerariae, RP). However, in its 2005 edition, the two species were separated into both individual monographs, namely 'Gegen' (Radix Puerariae Lobatae, RPL) and 'Fenge' (Radix Puerariae Thomsonii, RPT), respectively, due to their obvious content discrepancy of puerarin, the major active constituent. In present paper, the fingerprint of high-performance thin-layer chromatography (HPTLC) combining digital scanning profiling was developed to identify and distinguish the both species in detail. The unique properties of the HPTLC fingerprints were validated by analyzing ten batches of Pueraria lobata and P. thomsonii samples, respectively. The common pattern of the HPTLC images of the roots of Pueraria spp. and the respective different ratios of the chemical distribution can directly discern the two species. The corresponding digital scanning profiles provided an easy way for quantifiable comparison among the samples. Obvious difference in ingredient content and HPTLC patterns of the two species questioned their bio-equivalence and explained that recording both species separately in the current edition of Chinese Pharmacopoeia (2005 edition) is reasonable due to not only the content of major constituent, puerarin, but also the peak-to-peak distribution in the fingerprint and integration value of the total components. Furthermore, the HPTLC fingerprint is also suitable for rapid and simple authentication and comparison of the subtle difference among samples with identical plant resource but different geographic locations. 相似文献
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G. Du H.Y. Zhao Q.W. Zhang G.H. Li F.Q. Yang Y. Wang Y.C. Li Y.T. Wang 《Journal of chromatography. A》2010,1217(5):705-714
A microwave-assisted extraction (MAE) and ultra high performance liquid chromatography coupled with diode array detection and time-of-flight mass spectrometry (UHPLC-DAD-TOF-MS) method was developed for simultaneous determination of 14 phenolic compounds in the root of Pueraria lobata (Wild.) Ohwi and Pueraria thomsonii Benth. Operational conditions of MAE were optimized by central composite design (CCD). The optimized result was 65% ethanol as extraction solvent, 17 mL of extraction volume, 100 °C of extraction temperature and 2 min of hold time. A Zorbax SB C18 (50 mm × 4.6 mm I.D., 1.8 μm) and gradient elution were used during the analysis. The chromatographic peaks of 14 investigated compounds in samples were successfully identified by comparing their retention time, UV spectra and TOF mass data with the reference substances. All calibration curves showed good linearity (r > 0.9997) within the test ranges. The intra-day and inter-day variations were less than 1.77% and 2.88%, respectively. The developed method was successfully applied to determine the investigated compounds in 10 samples of Radix Puerariae Lobatae and Radix Puerariae Thomsonii, respectively. The result indicated that MAE and UHPLC-DAD-TOF-MS system might provide a rapid method for the quality control of Radix Puerariae. 相似文献
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Platycosides (PSs), the saponins found in the root of Platycodon grandiflorum (Jacq.) A. DC. (Platycodi Radix), are typically composed of oleanene backbones with two side chains; one is a 3-O-glucose linked by a glycosidic bond, and the other is a 28-O-arabinose-rhamnose-xylose-apiose linked by an ester bond. Minor saponins, acetylated isomers of the major saponin on either the 2' or 3' position of rhamnose, were isolated from Platycodi Radix using a multi-step process including high-speed counter-current chromatography (HSCCC) and preparative reversed-phase high-performance liquid chromatography (RP-HPLC). After the separation of the major components, the enriched minor saponin fraction was used for this study. A two-phase solvent system consisting of chloroform-methanol-isopropanol-water (3:2:2:3, v/v) was used for HSCCC. HSCCC separation of the enriched minor saponin fraction yielded 2'-O-acetylplatycodin D, 3'-O-acetylpolygalacin D, 2'-O-acetylpolygalacin and a mixture of 3'-O-acetylplatycodin D and polygalacin D. The mixture fraction from HSCCC separation was further purified by preparative RP-HPLC, giving 3'-O-acetylplatycodin D and polygalacin D at a purity of over 98.9%. The developed method provides the preparative and rapid separation of minor saponins in the crude extract of Platycodi Radix. To the best of our knowledge, this is the first on the separation of acetylated PSs by HSCCC. 相似文献
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Elution–extrusion counter‐current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix 下载免费PDF全文
Chu Chu Shidi Zhang Shengqiang Tong Xingnuo Li Qingyong Li Jizhong Yan 《Journal of separation science》2015,38(17):3110-3118
In this work, a simple and efficient protocol for the rapid separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix was developed by combining macroporous resin and elution–extrusion counter‐current chromatography. The crude extract was firstly subjected to a D101 macroporous resin column eluted with water and a series of different concentrations of ethanol. Then, effluents of 30 and 95% ethanol were collected as sample 1 and sample 2 for further counter‐current chromatography purification. Finally, a pair of isomers, 96 mg of compound 1 and 48 mg of compound 2 with purities of 91.1 and 96.2%, respectively, was isolated from 200 mg of sample 1. The other pair of isomers, 14 mg of compound 3 and 8 mg of compound 4 with purities of 93.6 and 88.9%, respectively, was isolated from 48 mg of sample 2. Their purities were analyzed by high‐performance liquid chromatography, and their chemical structures were identified by mass spectrometry and 1H NMR spectroscopy. Compared to a normal counter‐current chromatography separation, the separation time and solvent consumption of elution–extrusion counter‐current chromatography were reduced while the resolutions were still good. The established protocol is promising for the separation of natural products with great disparity of content in herbal medicines. 相似文献
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A silica gel column chromatography method is established for the isolation and purification of euparin and 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis. For the first time, a high-performance liquid chromatography (HPLC) method is developed to determine simultaneously two benzofurans with UV absorptions at 240 nm. The analysis is performed on a Diamonsil C?? column with a gradient solvent system of acetonitrile and aqueous phosphoric acid (0.2%, v/v) at a flow-rate of 1.0 mL min?1. All calibration curves reveal good linearity (r2 > 0.9998) within the tested concentration ranges. The relative standard deviations for intra-day and inter-day are less than 2.0% and the recoveries range from 98.32% to 103.68% with relative SDs less than 2.0%. This method is successfully applied to quantitate two benzofurans in Radix Eupatorii Chinensis. Therefore, the new HPLC method is proven to be reliable and suitable for the quality control of Radix Eupatorii Chinensis. 相似文献