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在碱性溶液中槲皮素对过氧化氢氧化鲁米诺而产生的化学发光(CL)具有很强的抑制作用,且其CL强度的减弱程度与槲皮素浓度之间在一定的范围内呈线性关系。据此,并结合应用流动注射(FI)技术,提出了FI-CL测定槐米中槲皮素含量的方法。反应体系中所用试剂的最佳浓度为:①cH2O2=0.2mol.L-1;②c鲁米诺=8.5×10-4mol.L-1;③cNaOH=0.01mol.L-1。对槲皮素测定的线性范围为2.65×10-6~5.31×10-4mol.L-1之间,其检出限(3s/k)为9.26×10-7mol.L-1。用4×10-4mol.L-1槲皮素标准溶液进行精密度试验,测得相对标准偏差(n=11)为3.0%。分析试样时,先从槐米在pH 8~9的碱性溶液中提取芦丁,然后在微酸性(pH 5)溶液中使芦丁水解得到槲皮素粗品。将此粗品经反复重结晶得到槲皮素纯品,溶于乙醇(40+60)溶液中制成溶液,用于FI-CL分析。 相似文献
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LIMin-jing YOUJing-yan YAOShuang DINGLan LIUZhong-ying ZHANGHan-qi 《高等学校化学研究》2004,20(6):703-706
Three microwave-assisted extraction(MAE) procedures were studied. The first procedure was household microwave oven dynamic extraction(HMODE). The second procedure was special microwave oven bath extraction (SMOBE). The third procedure was microwave resonant cavity dynamic extraction (MRCDE). The results obtained by the three microwave-assisted extraction procedures were compared with those obtained by using traditional Soxhlet extraction. The results indicate that the MAE not only took a shorter time, but also simplified the procedure, and made the extraction a higher yield. At the same time the results obtained by the three MAE procedures were also compared with each other. 相似文献
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金银花的毛细管电泳指纹图谱研究 总被引:23,自引:0,他引:23
采用毛细管区带电泳法,以50 mmol/L硼砂(含20 mmol/L β-环糊精(CD),用磷酸调pH 8.0)为背景电解质,运行电压12 kV,紫外检测波长254 nm,重力进样15 s(高度8.5 cm),建立了金银花药材水提取液的毛细管电泳指纹图谱(CEFP)。将13个不同产地的金银花药材供试液的CEFP进行比较,以电泳峰出现率100%计,确定金银花的共有指纹峰为18个。该CEFP具有较好的精密度和重现性,分离效能高且成本低廉。提出了指纹图谱宏观含量相似度R、投影含量相似度C和定量相似度P的概念,可从总体上评价药材化学组分的整体含量情况。从两个方面评价各产地药材与对照CEFP间的总体相似性,合格药材应具备以下两个条件:(1)代表化学成分分布相似性的定性相似度(S)≥0.90;(2)描述药材整体化学成分含量的定量相似度(R,C,P,Q)应在80%~120%。以此二类相似度指标控制金银花的质量,建立了指纹图谱评价的又一新方法。 相似文献
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红外光谱法与药用玫瑰真伪的分析与鉴定 总被引:4,自引:0,他引:4
文章采用红外光谱法(FTIR)并结合二维相关光谱分析技术分析鉴定了药用玫瑰(药材对照品)及其混淆品月季和蔷薇。在一维红外光谱中三者的谱图较为一致,但药用玫瑰在1 318 cm-1波数处的峰不明显 ,而月季和蔷薇的1 318 cm-1峰明显,且较尖。在高分辨的二阶导数谱中药用玫瑰和月季分别在1 617和1 618 cm-1处具有芳香类指纹特征峰,而蔷薇的峰则在1 612 cm-1波数处,相差了5~6 cm-1。在1 044 cm-1处的峰, 蔷薇糖类化合物的指纹特征峰较明显,月季和药用玫瑰不明显。观测二维相关红外谱,三者都存在1 620,1 560和1 460 cm-1的芳香类化合物的自动峰,不同的是月季和蔷薇还存在一个较明显的1 660 cm-1的肩膀峰。药用玫瑰、月季和蔷薇在850~1 250 cm-1范围内的二维相关红外光谱差别很大,药用玫瑰1 050 cm-1的糖类化合物自动峰强度最大,而月季的峰较弱,而蔷薇没有此峰。谱图的三级鉴定验证了药用玫瑰、月季和蔷薇在糖苷类化合物和芳香类化合物的相对含量上都是不一致的。结果表明,运用红外光谱法可以快速有效地分析和鉴定药用玫瑰及其混淆品。 相似文献
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Yuhui Wei Boxia Li Haogang Duan Xin'an Wu Xiaojun Yao 《Biomedical chromatography : BMC》2010,24(3):289-293
A large number of herb materials contain essential oils with extensive bioactivities. In this work, an integrated simultaneous distillation–extraction (ISDE) apparatus was developed. To demonstrate its feasibility, the performance of ISDE was evaluated for the extraction of essential oil from Flos Magnoliae and compared with conventional techniques including steam distillation (SD) and simultaneous distillation–extraction (SDE). According to the product yield, the time consumed and the composition of oil, the essential oils isolated by ISDE were better than that obtained by SD and similar to those obtained by SDE. ISDE was also better than SDE due to its simple operation and lower consumption of energy and organic solvent. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
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Tracing novel hemostatic compounds from heating products of total flavonoids in Flos Sophorae by spectrum–effect relationships and column chromatography 下载免费PDF全文
Hao Wu Yaozong Pan Kuilong Wang Liping Liu Yangping Jin Chenchao Zhang 《Journal of separation science》2015,38(10):1691-1699
Flos Sophorae and its processed product have been clinically used to treat hemorrhage. In this study, the total ion chromatographic fingerprints of the heating products of total flavonoids in Flos Sophorae were established by high‐performance liquid chromatography with tandem mass spectrometry and the hemostatic activities were studied by hemostatic screening tests in vivo. The spectrum–effect relationships between fingerprints and hemostatic activities were investigated using canonical correlation analysis to trace the peaks responsible for the hemostatic effects. The predicted active peaks in fingerprints were isolated by column chromatography and their structures were identified by NMR spectroscopy and mass spectrometry. The hemostatic activities of them were verified by platelet aggregation and procoagulation assays in vitro. Canonical correlation analysis results showed that peak 8 and peak 11 were correlated most closely, thus probably being the main hemostatic compounds. Through column chromatography separation, peak 8 (compound I) and peak 11 (compound II) were obtained with purities of 95.61 and 93.38%, respectively, and were discovered new hemostatic compounds named as huaicarbon A (I) and huaicarbon B (II), respectively. This study provides a universal model to trace the active compounds of other herbs which have bioactivity enhancement after processing by spectrum–effect relationships and column chromatography. 相似文献
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以金银花为试材,研究了叶面喷施稀土镧对金银花中重金属及药效成分含量的影响。结果显示以过氧化物酶活性和叶绿素含量为指标,确定以30 mg·L-1的甘氨酸镧水溶液叶面喷施效果较好。30 mg·L-1的甘氨酸镧水溶液处理的金银花中,Cd,Cu和As含量与对照相比明显下降,同时药效成分绿原酸和木犀草苷的含量分别增加了9.14%和43.86%。与药典标准相比,重金属含量和药效成分含量都明显优于2010版药典标准。结果表明:适宜浓度稀土镧对金银花吸收重金属元素有抑制作用,并且能促进其药效成分的合成,进而提高金银花的品质。 相似文献
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Comprehensive two-dimensional liquid chromatographic separation by means of a combination of ion-exchange chromatography (IEC)
and reversed-phase liquid chromatography (RPLC) has been realized and applied to the analysis of components of a traditional
Chinese medicine Flos Lonicera. In the first dimension the components of a Flos Lonicera extract is separated on strong anion-exchange (SAX) column according to the charge-exchange properties of the components.
In the second dimension the components are further fractionated by reversed-phase liquid chromatography (on ODS) on the basis
of their hydrophobicity. The RPLC effluent is desalted and split and the components are identified on-line by use of both
diode-array detection and mass spectrometry with atmospheric pressure chemical ionization (APCI–MS). In this way, the extract
of Flos Lonicera can be rapidly separated, desalted, and analyzed, with determination of molecular weight. More than 58 components of an extract
of Flos Lonicera were well resolved and six were tentatively identified from their UV and mass spectra. 相似文献