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红景天甙和红景天甙元标准品的制备方法研究 总被引:5,自引:0,他引:5
用化学和高效液相制备色谱方法分离制备了红景天属植物提取物中甙及甙元的标准物,标准品纯度分别由1%~2%和1%提高到99%和97%以上。 相似文献
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毛细管电泳测定三精双黄连口服液中的黄芩甙元、黄芩甙、绿原酸和咖啡酸 总被引:3,自引:1,他引:2
建立了毛细管电泳法测定中药复方制剂双黄连口恨液中黄芩甙元、黄芩甙、绿原酸和咖啡酸的方法,通过研究缓冲溶液pH和浓度、分离电压、进样时间和有饥添加剂的影响优化了分析条件在优化的条件下,20min内实现了4种物质的良好分离黄芩甙元、黄芩甙、绿原酸和咖啡酸峰高和质量浓度分别在0.05~1.50、0.06~1.20、0.02~0.50和0.02~0.50g/L范围内呈良好线性;俭出限分别为0.015、0.020、0.004、0.004g/L基于迁移时间和峰高的重复性分别为:黄芩甙元,1.70%和3.94%;黄芩甙,1.60%和3.63%;绿原酸,1.60%和2.05%;咖啡酸,1.51%和2.83%通过分析实际样品并做加标回收实验验证了该方法的可行性。 相似文献
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苦杏仁甙化学发光生物传感器 总被引:7,自引:0,他引:7
将具有分子识别功能的β-葡萄糖甙酶和能进行换能反应的Luminol分别固定在壳质胺和大孔阴离子交换剂的柱中,组成流动注射系统。苦杏仁甙在β-葡萄糖甙酶催化下分解生成的CN^-(分子识别反应)与溶解氧反应生成超氧阴离子自由基,继而同Luninl反应产生化学发光(换能反应)。这一新型生物传感器的化学发光强度与苦杏杜甙量在1~200ug之间呈良好线性关系,检出限为0.3ug,相对标准偏差为3.1%,并具 相似文献
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制备型高效液相色谱法从积雪草提取物中分离纯化积雪草甙和羟基积雪草甙对照品 总被引:2,自引:0,他引:2
积雪草甙和羟基积雪草甙是积雪草及其相关制品质量控制的两个指标成分,本研究利用制备型高效液相色谱从积雪草提取物中同 时分离纯化得到这两个成分。对制备色谱的流动相组成、流速、进样量和检测波长等制备参数进行了优化。采用的色谱柱为C18柱(50 mm×200 mm,5 μm);流动相为甲醇-水(体积比为60∶40),流速100 mL/min;二极管阵列检测器在220 nm检测;进样体积为1.5 mL。在20 min的运行时间内,积雪草甙和羟基积雪草甙与干扰成分得到很好的分离,产品纯度达到98%以上。此方法具有快速高效、产品纯度高的 特点,可以用于制备积雪草甙和羟基积雪草甙对照品。 相似文献
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通过测定产物间接测定扁桃甙,如用酶修饰电极测定产物氢氰酸和葡萄糖,其检测限均在10~(-5) mol/L。本文首次采用卷积伏安法研究了扁桃甙的水解以及产物苯甲醛的极谱行为,提高了扁桃甙的检测限。 1 仪器与试剂 XJP-821型新极谱仪(长春应用化学研究所、江苏电分析仪器厂),三电极体系,LZ3-100 相似文献
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牛蒡叶中微量木脂体牛蒡子甙和牛蒡子甙元的分离与鉴定 总被引:7,自引:0,他引:7
建立了分离鉴定牛蒡叶中微量木脂体牛蒡子甙(arctiin)和牛蒡子甙元(arctigenin)的方法。牛蒡叶粗提物经聚酰胺柱提取,浓缩其甲醇洗脱液并于低温下静置析出白色沉淀物。沉淀物用甲醇溶解后经反相高效液相色谱(RP-HPLC)分离,纯化得到两个主要组分。经紫外光谱(UV)、红外光谱(FTIR)及电喷雾质谱(ESI-MS)检测,并与牛蒡子甙和牛蒡子甙元对照品的UV,LC-ESI-MS,HPLC及FTIR图谱比较,鉴定两个主要成分为牛蒡子甙和牛蒡子甙元。 相似文献
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重结晶法分离精制莱鲍迪甙A的研究 总被引:4,自引:0,他引:4
用甲醇、异丙醇和水不同比例的混合溶剂对甜叶菊糖以及分离出甜菊甙的母液浓缩物分别进行重结晶研究,考察了甜菊甙和莱鲍迪甙A的结晶分离及菜鲍迪甙A结晶纯化的最佳条件,得到了高纯度的莱鲍迪甙A,并对其进行了熔点测定和HPLC表征,为莱鲍迪甙A的分离与纯化提供了一种简便的方法。 相似文献
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树脂吸附层析法分离喜树果中的喜果甙 总被引:3,自引:0,他引:3
自 1 96 6年 Wall等 [1] 首次从喜树植物中分离出喜树碱后 ,至今已有 2 0多种化学成分从中分离出来 ,包括喜树碱 (Camptothecine,CPT)、 1 0 -羟基喜树碱、 1 1 -羟基喜树碱、 1 0 -甲氧基喜树碱、喜树次碱、白桦脂酸及喜果甙 (Vincoside- lactam,VCS- LT)等 [2 ] .研究表明 ,喜树碱类化合物和喜果甙均具有抗癌活性 [3~ 5] .从喜树果中分离喜果甙对充分利用我国丰富的喜树资源具有重要意义 .目前文献报道的分离提取喜果甙方法主要是溶剂萃取和氧化铝柱层析法 [6] ,过程复杂 ,收率很低 .本文采用树脂吸附法对喜果甙进行分离纯化 ,再经… 相似文献
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We elucidated the structure and metabolite profile of eleutheroside B, a component derived from the extract of Acanthopanax senticosus Harms, after oral administration of the extract in rats. Samples of rat plasma were collected and analyzed by selective high‐resolution liquid chromatography/quadrupole time‐of‐flight mass spectrometry (UPLC/Q‐TOF MS) automated data analysis method. A total of 11 metabolites were detected: four were identified, and three of those four are reported for the first time here. The three new plasma metabolites were identified on the basis of mass fragmentation patterns and literature reports. The major in vivo metabolic processes associated with eleutheroside B in A. senticosus include demethylation, acetylation, oxidation and glucuronidation after deglycosylation. A fairly comprehensive metabolic pathway was proposed for eleutheroside B. Our results provide a meaningful basis for drug discovery, design and clinical applications related to A. senticosus in traditional Chinese medicine. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Colas C Popot MA Garcia P Bonnaire Y Bouchonnet S 《Biomedical chromatography : BMC》2008,22(8):912-917
LC/ESI-MS n methods have been previously set up to detect the administration of (i) Harpagophytum and (ii) preparations containing a plant capable of anti-stress properties: Eleutherococcus senticosus. Harpagoside has been found to be the main indicator of Harpagophytum administration in the horse. These methods have been applied to a large number of horse urine samples of various origins. Regarding the detection of Harpagophytum administration, harpagoside, harpagide and 8-para-coumaroyl harpagide were detected together in only one sample out of 317. Eleutheroside E was found to be the main indicator of Eleutherococcus senticosus administration. It was detected in post-administration samples collected from two horses having received a feed supplement containing Eleutherococcus senticosus for several days. Out of the 382 samples tested, eleutheroside E was found in an unexpected large number of urine samples (39%) of various origins and its presence cannot be only due to the sole use of herbal dietary supplements. 相似文献
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A method for the isolation, purification, and determination of eleutheroside E in Acanthopanax giraldii Harms, collected in the Sichuan province (China), is established. The water extraction of A. giraldii Harms is pre-isolated using macroporous adsorption resin (D-101) and a C18 solid-phase extraction cartridge, and the enriched extract is purified to give eleutheroside E (syringaresinol-di-O-beta-D-glucoside; liriodendrin) by semipreparative reversed-phase high-performance liquid chromatography. Structure identification is performed by a comparison of IR, 1H-NMR, 13C-NMR, and electrospray ionization-mass spectrometric data with the literature. The final purity of the compound is 97%. Quantitative determination of eleutheroside E in A. giraldii Harms is performed on a Zorbax SB C18 (150- x 4.6-mm i.d., 5 microm) column. The linear range of eleutheroside E is 4.85-194 mg/L (r = 0.9998), and the average recovery is 99.6-101%. The developed method is simple, reproducible, and easy to operate. It is useful for the evaluation of Acanthopanax giraldii Harms. 相似文献
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Summary The complete structures of eleutherosides I, K, L, and M have been established. Glycoside I is identical with mubenin B and glycoside M with hederasaponin B. It has been shown that eleutheroside K is the 3-[O--L-rhamnopyranosyl-(1»2)--L-arabopyranoside] of oleanolic acid. In eleutheroside L, the L-rhamnose and L-arabinose residues are connected by a 1»4 bond, and a trisaccharide consisting of O--L-rhamnopyranosyl-(1»4)-O--D-glucopyranosyl-(1»6)--D-glucopyranose is connected with the carboxy group.Institute of Biologically Active Substances of the Far-Eastern Scientific Center of the Academy of Sciences of the USSR. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 618–622, September–October, 1971. 相似文献
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Yu. S. Ovodov G. M. Frolova L. A. Elyakova G. B. Elyakov 《Russian Chemical Bulletin》1965,14(11):2035-2036
Summary It was shown that eleutheroside E, one of the glycosides isolated from the prickly eleutherococcus, is identical with acanthoside D, which is one of the glycosides isolated from the cluster-flowering acanthopanax and represents the. di--D-glucoside of (–)-syringaresinol.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 11, pp. 2065–2067, November 1965 相似文献
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From the whole plant of Sarcandra glabra, a new phenolic acid glycoside, benzyl 2-β-glucopyranosyloxybenzoate (1), together with seven known compounds including eleutheroside B? (2), 5-O-caffeoylshikimic acid (3), (-)-(7S, 8R)-dihydrodehydrodiconiferyl alcohol (4), (-)-(7S, 8R)-dihydrodehydrodiconiferyl alcohol 9-, 9′- and 4-O-α-D-glucopyranoside (5-7), and (-)-(7S, 8R)-5-methoxydihydrodehydrodiconiferyl alcohol 4-O-β-D-glucopyranoside (8) was isolated. Their structures were elucidated by spectral analysis including 1D-, 2D-NMR and HR-ESI-MS. Compound 2 was found to exhibit potent cytotoxic activity against BGC-823 and A2780 cancer cell lines using MTT method with IC?? value of 2.53 and 1.85 μM, respectively. 相似文献
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Nakamura S Zhang Y Matsuda H Ninomiya K Muraoka O Yoshikawa M 《Chemical & pharmaceutical bulletin》2011,59(8):1020-1028
The methanolic extract from the leaves of Salacia chinensis collected in Thailand was found to show a protective effect on D-galactosamine-induced cytotoxicity in primary cultured mouse hepatocytes. From the methanolic extract, eight new glycosides, named foliachinenosides E, F, G, H, and I, and foliasalaciosides J, K and L, were isolated together with 26 known constituents. The structures of new glycosides were determined on the basis of physicochemical and chemical evidence. In addition, the hepatoprotective effects of the isolated compounds on D-galactosamine-induced cytotoxicity were examined. Among them, lignans, eleutheroside E? and 7R,8S-dihydrodehydrodiconiferyl alcohol 4-O-β-D-glucopyranoside, were found to show the protective effects [inhibition (%) 41.4 ± 3.6 (p < 0.01), 45.5 ± 2.7 (p < 0.01) at 100 μM, respectively]. 相似文献
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目前中药制剂生产过程中缺乏全过程参数检测和质量控制技术手段,不同生产批次药品化学成分差异较大、质量不够稳定、临床使用疗效和安全性不理想,因此,建立其完善的质量评价体系及其准确快速的质量评价方法,成为中药质量控制的重中之重.通过对刺五加注射液近红外(near infrared,NIR)含量预测模型的谱段选择规律和消除溶剂干扰方法的探讨,发现采用表征混合物结构差异的结构相关谱段结合含量相关谱段作为NIR组分预测模型谱段,用基于水为参比光谱的样本光谱建立含量预测模型,并利用水作为参比光谱识别和提取待分析组分的光谱信息,可以得到较理想的NIR含量预测结果.通过对刺五加注射液中绿原酸、紫丁香苷和刺五加苷E组分的近红外光谱结构相关谱段和含量相关谱段的归属,分别建立了绿原酸、紫丁香苷和刺五加苷E组分的含量预测模型,可用于快速分析刺五加注射液中不同组分的含量. 相似文献