灯盏生脉胶囊的鉴别研究

目的：完善灯盏生脉胶囊的薄层鉴别．方法：采用薄层鉴别以野黄芩苷、五味子乙素为对照品。结果：供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的荧光斑点。结论：方法专属、斑点清晰、分离度好,可用于灯盏生脉胶囊的薄层鉴别。     

Rapid TLC determination of methadyl acetate and some in vitro metabolites.

Methadyl acetate was metabolized by microsomal preparations of rat liver to yield nor-methadyl acetate and 6-(dimethylamino)-4,4-diphenyl-3-heptanol. The identification and separation of these three compounds was established by TLC, using iodoplatinate spray as a visualizing agent.     

Historical study of separation technology innovation in the field of pharmaceutical science

The separation of organic compounds has been carried out using the method of distillation and recrystallization since the 17th century.1st separation technology innovation (1950s to 1960s). After World War II, the science of separating organic compounds evolved to the use of paper or column chromatography. 2nd separation technology innovation (1960s to 1980s). In the 1960s, thin-layer chromatograpy (TLC) was developed. TLC is a convenient analytical technique for organic compounds. Separation methods for organic compounds using column chromatography and preparative TLC were carried out as practical applications. Gas chromatography (GC) was also introduced in the 1960s. GC is a useful analytical method for a mixture of various volatile organic compounds. Many GC instruments with new kinds of sensors were developed. Gas chromatography of nonbenzenoid organometallic compounds and metal complexes was successfully conducted by the author. 3rd separation technology innovation (1980s to 1990s). In the 1980s, high-performance liquid-chromatography (HPLC) was developed. HPLC analytical methods were useful for various kinds of organic compounds. In the 1990s, LC-MS and LC-NMR instruments were introduced for biomedical products. 4th separation technology innovation (1990s to present). Several new ionization methods for mass-spectrometry (electrospray, matrix-aided lazer desorption ionization, etc) are applied for proteins and biomedical products. Several new separation technologies (supercritical field chromatography, capillary electrophoresis, field-flow fractionization, etc.) are now being developed.     

中药点滴荧光鉴别法的研究

目的该文诣在建立一种适用于基层的,快速便捷的中药点滴荧光鉴别法。方法在紫外灯下对药材粉未及滴加常用试剂后的荧光进行观察,配以数码摄影,并利用电脑对其荧光斑点进行色彩分析,得出药材荧光斑点的颜色数据,以此作为鉴别和证据。结果与结论实验表明,该方法的稳定性、重现性、精密度均较好,在中药材的真伪上有一定意义。     

Controlled biosynthesis of neoviridogriseins, new homologues of viridogrisein. III. Production, structures and biological properties of neoviridogriseins I and III

The high response of our isolate of Streptomyces griseoviridus was exploited to provoke the synthesis of new viridogrisein homologues by adding various amino acids to the culture medium in an attempt to replace the alanine, sarcosine, leucine and phenylsarcosine moieties of virdogrisein. Among the amino acids added, L- and DL-alpha-amino-n-butyric acid and L-methionine gave new TLC spots which we named neoviridogriseins I and III and neoviridogrisein VII, respectively. The structures of neoviridogriseins I and III were elucidated: In both compounds, the alanine moiety of viridogrisein is replaced by a L-alpha-amino-n-butyric acid residue; furthermore, in neoviridogrisein I, the allo-hydroxy-D-proline is replaced by D-proline.     

云芝的薄层色谱鉴别

目的 建立云芝的薄层色谱鉴别方法.方法 以环己烷-三氯甲烷-甲酸乙酯-水(8∶7∶5∶1)为展开剂,用硅胶G预制薄层板,以10%的硫酸乙醇液为显色剂,进行薄层色谱分析.结果 云芝与云芝对照药材在薄层板上主斑点位置及颜色一致,且斑点集中、分离度好.结论 所建立的方法快速、简便、灵敏、重现性好、专属性强,可以作为云芝的质量控制方法之一.     

Fluorescence--TLC densitometric determination of diazepam and other 1,4-benzodiazepines in serum.

A sensitive fluorescence--TLC densitometric procedure was developed for the specific determination of diazepam (I) and its two metabolites, desmethyldiazepam (II) and oxazepam (III), in serum. After extraction from serum with benzene, the compounds were separated by TLC and converted with a sulfuric acid spray to greenish-yellow fluorescence spots with Rf values of 0.72, 0.43, and 0.17, respectively. Quantitation of the TLC plate was accomplished by scanning with a densitometer at 380 nm. The sensitivities of the assay were 18 (I), 6 (II), and 5 (III) ng/ml of serum. This procedure was also was applicable to other 1,4-benzodiazepines in biological fluids.     

常用中药材的荧光观察

采用在紫外灯下数码摄影的方法,对药材粉未及滴加常用试剂后的荧光进行观察,并利用电脑对其荧光斑点进行色彩分析,得出各药材荧光斑点的颜色数据。结果在315种常用药材中,约3/4有一定强度的荧光反应。表明荧光鉴别在中药鉴定上具有普遍意义。     

紫草总色素β-环糊精包合物的定性鉴别及左旋紫草素含量测定

目的建立定性鉴别紫草总色素β-环糊精包合物有效成分的薄层色谱(TLC)法和测定左旋紫草素含量的高效液相色谱(HPLC)法。方法采用TLC法进行定性鉴别,展开系统为环己烷-甲苯-乙酸乙酯-甲酸(5∶5∶0. 5∶0. 1,V/V/V/V);采用HPLC法测定包合物中有效成分左旋紫草素的含量,流动相为甲醇-0. 025 mol/L磷酸(82∶18,V/V)。结果 TLC鉴别中,供试品溶液与对照品溶液在相应位置上显相同颜色斑点,且斑点清晰,阴性对照无干扰;HPLC图中,供试品溶液与对照品溶液色谱出峰时间一致,分离度好,阴性对照无干扰,含量测定中有效成分的线性关系良好,平均加样回收率为102. 09%,RSD为1. 87%(n=6)。结论该方法操作简便、结果准确、专属性强、重复性好,可用于该产品的质量控制。     

离心薄层层析法分离半合成头孢菌素衍生物的研究

本文用离心薄层层析法对半合成头孢菌素类化合物进行了制备量分离的研究。采用此法有效地分离了Ⅱ、Ⅲ两个系列共38个半合成头孢菌素衍生物,深入探讨了吸附层、洗脱剂、分离样品限量、分离时间等分离条件。结果表明:离心薄层层析法适用于半合成头孢菌素的分离,仪器简单,操作方便,经济省时,具有满意的分离效果。     

Solid-supported reagents for multi-step organic synthesis: preparation and application

Since the early days of combinatorial chemistry solid-phase organic synthesis has been the method of choice for the production of large libraries. Solution-phase synthesis is again gaining importance especially for the synthesis of parallel arrays of smaller, focussed libraries containing single compounds with high degrees of purity. In the field of solution-phase library generation, the use of solid-supported reagents, catalysts and scavengers is emerging as a leading strategy, combining the advantages of both solid-phase organic synthesis (e.g. allowing the employment of an excess of reagent without the need for additional purification steps) and solution-phase chemistry (e.g. the ease of monitoring the progress of the reactions by applying LC-MS, TLC or standard NMR techniques). An account of some of the most recent advances in this area of research will be presented.     

藏药“俄色”的薄层色谱研究

目的:建立藏药"俄色"的薄层色谱鉴别方法。方法:通过对提取试剂及展开系统进行系统的考察,建立以根皮素对照品为对照、以氯仿-甲醇-甲酸(8:2:0.1)为展开系统的薄层色谱鉴别方法。结果:不同批次俄色药材在与对照色谱相应的位置上,显相同颜色的荧光斑点,能够有效的对"俄色"进行鉴别。结论:首次建立了藏药"俄色"的薄层鉴别方法,该方法的Rf值适中,斑点清晰,具有较好的适应性,重现性好,为完善其质量标准奠定了基础。     

玉叶清火胶囊中玉叶金花鉴别方法的研究

目的:考查玉叶清火胶囊中玉叶金花的鉴别方法。方法:通过改变提取方法、洗脱剂、展开剂选择薄层色谱法(TLC)中的最佳实验条件。结果:经大孔树脂处理,20%～30%之间的乙醇洗脱,以三氯甲烷-甲醇-水(13:6:2)10℃以下放置分层的下层溶液为展开剂得到的薄层色谱图中,玉叶金花与对照药材色谱在相应的位置上,显相同颜色的斑点,且斑点清晰,分离效果好,阴性对照无干扰。结论:实验证明此方法简便、快捷,能准确鉴别出玉叶清火胶囊中的玉叶金花。     

胃乐舒颗粒的质量控制

目的:建立胃乐舒颗粒的质量控制方法。方法:采用薄层鉴别法(TLC)对制剂中主要药味延胡索、旋覆花、山楂、厚朴进行定性鉴别;以HPLC法测定延胡索中延胡索乙素的含量:色谱柱为Agilent SB-C₁₈(4.6 mm×250 mm,5 μm),流动相为乙腈-0.1%磷酸溶液(45:55,磷酸溶液用三乙胺调pH到6),检测波长为226 nm。结果:在薄层色谱中,各供试品色谱,在与对照品或对照药材相应的位置上显相同颜色的斑点,阴性对照无干扰;延胡索乙素在0.050~0.657 μg范围内线性关系良好,r=1.000 0。结论:该方法操作简单,重复性好,能够有效地控制胃乐舒颗粒的质量。     

Coloration of phenothiazines with metal-containing drugs

We studied the color change of phenothiazines and metal-containing drugs after compound formation, followed by use of FT-Raman spectrocopy to observe any structural changes in them. When 6 phenothiazines (thioridazine hydrochloride, prochlorperazine maleate, levomepromazine maleate, chlorpromazine phenolphthalinate, fluphenazine maleate and perphenazine fendiate) formed compounds with natural aluminum silicate, the color change was accompanied by a shift of FT-Raman signals. These changes could be attributed to the structural changes of phenothiazines. This present observation can be then used in advance to avoid coloration of phenothiazines during preparative procedures with metal-containing drugs such as antacids.     

TLC fractionation and visualization of selected phenolic compounds applied as drugs

Sixteen visualizing agents, thirteen of which were a group of alkacemetric indicators were used for the detection of selected drugs (being phenolic compounds): adrenaline, dopamine, phenylephrine, metaraminol, fenoterol, and bithionol. Visualizing effects for the drugs investigated after their TLC separation were estimated on silicagel (A), mixture silica gel/kieselguhr (B), and on polyamide (C). The best separations and the most positive visualising effects were obtained on adsorbent A, and the least on absorbent C. On adsorbent A, the most profitable detectability equal to 100 ng, was obtained also for adrenaline, dopamine and fenoterol with the application of basic solution of bromocresol green and brilliant cresyl blue as visualizing agents.     

金果饮的质量控制研究

目的：对金果饮的质量标准进行制定。方法：对玄参、西青果、陈皮建立薄层色谱的鉴别方法;采用高效液相色谱法测定橙皮苷的含量。用Agilent SB C18柱（4.6mm×250mm,5μm）,以甲醇-6%乙酸溶液（35∶65）为流动相;检测波长为283nm,流速1mL·min-1。结果：薄层色谱鉴别中,供试品在与对照药材色谱相应的位置上,显示相同颜色的斑点,斑点清晰,分离效果好,阴性无干扰;含量测定法中,橙皮苷在36.35～726.95ng（r=0.9999,n=5）范围内呈良好的线性关系,平均加样回收率为98.58%（RSD为1.85%）。结论：建立的方法简便、准确、专属性强、重复性好,能有效用于金果饮的质量控制。     

Examination of iron (III) and hexacyanoferrate (III) ions as reagents for the spectrophotometric determination of promazine and perazine

Iron (III) chloride and potassium hexacyanoferrate (III) have been tested as reagents for the determination of promazine hydrochloride and perazine. The methods are based on the oxidation of phenothiazines by FeCl3 and K3[Fe(CN)6] in perchloric acid medium. The optimal conditions for the formation of oxidation products of promazine and perazine were examined. The absorption spectra in the UV-VIS region were recorded.     

多种药材的增荧光薄层鉴别研究

目的拓宽薄层鉴别检测途径,提高中药成方制剂中的薄层鉴别增订率。方法将各药材的样品溶液点于薄层板上,展开后,进行不同方式的增荧光反应研究。结果药材中多种无检测信息的成分呈现出不同颜色的荧光,斑点清晰,检测灵敏度提高,信息量增大。结论本研究有效拓宽了薄层鉴别检测途径,使多种无检测信息的中药材,能够被高灵敏度、准确地进行定性和定量控制。     

Struktur der Produkte aus Cotarnin und Hydrastinin mit CH-aciden Verbindungen und Acetanhydrid

Structure of the Products of Reactions of Cotarnine and Hydrastinine with CH Acidic Compounds and Acetic Anhydride The products resulting from reactions of cotarnine and hydrastinine with CH acidic compounds are cyclic derivatives with substituents at position 5. The reaction of carbinolamines with acetic anhydride causes ring opening. Cyclic ?O-acetylcotarnine”? was identified as the opened-chain acetylcotarninacetic acid.