黄麻链霉菌NF0919菌株发酵液有效成分薄层色谱分离的展开剂优化

根据单因素试验法确定了黄麻链霉菌(Streptomyces corchorusii)NF0919菌株发酵产物的薄层色谱展开剂组分,利用均匀设计法和逐步回归法建立回归模型优化展开剂的配比,最终得出最优化的展开剂系统为氯仿一甲醇一水一冰醋酸=10∶2.75∶0.5∶0.2,分离效果较理想。     

葛根异黄酮的快速分离检测方法研究

以SDS正丁醇-正庚烷-水组成的微乳体系作为展开剂,通过聚酰胺薄层层析,探讨不同类型微乳液对葛根异黄酮分离检测效果的影响。结果表明,选择含水量为70％的微乳液作为展开剂,分离效果明显,一次检测出12个黄酮化合物;与以三氯甲烷-甲醇-水(7:2．5:0．25)为展开剂的硅胶薄层相比,微乳薄层色谱对葛根异黄酮的检测效果和灵敏度显著提高,为实验研究中常规检测提供了简便快捷的方法。     

野葛花中葛花苷的测定方法研究

在硅胶G薄层色谱板上,建立了双波长薄层扫描法测定野葛花中葛花苷的分析方法。薄层分析的展开剂为三氯甲烷一甲醇一冰醋酸(3：1：0．3)．葛花苷在0．484～3．872μg范围内呈良好线性。该方法快速、简便,为野葛花作为中药质量控制提供科学依据。     

无患子及其制剂的薄层色谱鉴别探讨

目的探讨无患子及其制剂的鉴别方法。方法采用薄层色谱法在不同条件下进行薄层色谱考察,选择适宜的薄层色谱条件。结果最佳薄层色谱条件为:以正丁醇-乙酸乙酯-水-浓氨水(40∶10∶50∶1;V∶V∶V∶V)上层液为展开剂,室内环境中展开,晾干,喷5%磷钼酸乙醇液,105℃加热至斑点清晰,在日光下检视,无患子及其在制剂中的成分分离效果良好,色谱斑点清晰,耐用性好。结论该法操作简便可靠,分离度较好,可作为无患子及其制剂的鉴别方法。     

藏药婆婆纳药材薄层鉴别方法学研究

本文建立了藏药婆婆纳药材的薄层鉴别方法。采用单因素试验方法,对影响婆婆纳对照药材的薄层色谱因素进行系统考察,筛选出最佳的薄层色谱条件。该薄层鉴别条件吸附剂:硅胶G薄层板;展开剂:环己烷-丙酮(6∶4);显色剂:10%硫酸乙醇溶液;显色条件:110℃烘箱中加热至斑点显色清晰,日光下检视,所得的薄层色谱,斑点清晰,分离度好。该方法分离度高,重现性好,简便,可用于婆婆纳的质量控制。     

苦杏仁对照提取物替代苦杏仁对照药材的可行性研究

目的：以对照药材技术要求为基础,以等量同质为原则,利用现代的提取制备技术,制备成质量稳定、均匀性好的苦杏仁对照提取物。通过考察不同的薄层系统,建立薄层鉴别用对照提取物的质量标准,供中药标准中薄层鉴别使用。并对其主要药效成分进行方法学考察,确保今后制备的对照提取物的一致性。方法：采用不同薄层色谱系统对苦杏仁对照提取物可替代对照药材进行定性研究;并用高效液相色谱法测定苦杏仁对照提取物中苦杏仁苷的含量。结果：在苦杏仁对照提取物薄层色谱中,展开剂：为甲苯－甲酸乙酯－甲醇－甲酸－水（6∶2∶0．4∶0．1∶0．1 ）,在与对照药材色谱相应位置上,显相同颜色的斑点。HPLC测定苦杏仁对照提取物中苦杏仁苷含量,苦杏仁苷线性范围461．7～15．39 mg／L（r＝0．9995）,平均回收率为101 ．1％（RSD＝2．15％）,该方法准确、可靠、专属性强,重复性好。结论：苦杏仁对照提取可替代对照药材进行定性鉴别。     

蔓荆子中紫花牡荆素和对羟基苯甲酸的吸附薄层色谱分析

本文用吸附薄层色谱分析分离蔓荆子时,优化了展开剂,结合薄层扫描仪,建立了系统定量测定蔓荆子中紫花牡荆素和对羟基苯甲酸的分析方法,回收率试验满意。     

反相薄层色谱扫描方法分离蟾酥成分及测定脂蟾毒配基含量

本文用 BC_(18)F_(254)板,乙腈-水(1:1)作展开剂,展开8cm。反相薄层色谱扫描法分离并检测蟾酥中的八个成分,其中脂蟾毒配基的定性、定量方法已被建立。并用此法测定了三个蟾酥样品中脂蟾毒配基的含量。平均回收率为103.8％,变异系数(CV)小于2％,比现有其它方法重视性好,分离效率高,操作简便。     

治糜灵凝胶剂的薄层色谱鉴别研究

目的:将治糜灵栓剂(《中国药典》2010版一部)改为治糜灵凝胶剂,建立治糜灵凝胶剂的薄层色谱鉴别方法,为制定其质量控制标准制定依据。方法:参照《中国药典》2010版一部治糜灵栓剂项下黄柏、苦参、儿茶、冰片的薄层色谱鉴别方法,对处方中的主要药味进行定性鉴别。黄柏鉴别中以甲苯-乙酸乙酯-异丙醇-水(6:3:1.5:1.5)为展开剂;苦参鉴别中以甲苯-乙酸乙酯-甲醇(8:3:0.5)为展开剂;儿茶鉴别中以正丁醇-醋酸-水(3:2:1)为展开剂;冰片鉴别中以环己烷-三氯甲烷-乙酸乙酯(9:1:2)为展开剂。结果:薄层色谱上具有黄柏,苦参,儿茶,冰片的鉴别特征,且阴性对照无干扰。结论:色谱斑点清晰,专属性强;该方法操作简便,稳定性、重现性均很好。可作为质量标准的控制依据。证明治糜灵凝胶剂研究的方法可行。     

右旋磷霉素手性转化产物检测方法的建立

建立以右旋磷霉素为底物生物转化产生左旋磷霉素的检测方法。通过考察藤黄微球菌与大肠埃希菌对左旋磷霉素的最小抑菌浓度,确定检定菌种类;优化薄层色谱展开剂系统,将薄层色谱与生物显影相结合对转化产物进行定性;利用含量标准曲线,使用生物活性检测法对转化产物进行定量。藤黄微球菌对左旋磷霉素的最小抑菌浓度比大肠埃希菌小100倍,因此作为本实验的检定菌;薄层色谱的最佳展开剂确定为正丁醇/甲醇/水(4∶3∶2,体积比),此时左旋磷霉素在生物检定板上呈现边缘清晰的抑菌圈,且Rf值为0.51;在1.43~5.0 mg/mL范围内,抑菌圈直径与磷霉素浓度的对数值成正比。以藤黄微球菌作为检定菌,不需要对转化产物进行分离纯化和精制,可利用薄层色谱与生物显影相结合的方法对产物进行定性,利用生物活性检测法对产物进行定量,达到简便快速地对转化产物进行定性和定量的目的。     

栀子黄色素制备藏红花酸研究

以栀子黄色素为原料,对其水解反应制备藏红花酸及其纯化条件进行了研究,结果表明,栀子黄色素经碱水解法制备藏红花酸的最佳条件为:KOH溶液10%、温度为60℃、反应时间120 min,水解所得藏红花酸通过甲醇除杂,重结晶后,所得结晶其mp.、uv与文献报道一致,其质谱的诱导碰撞解离技术获得碎片裂解信息均表明所得到的结晶为藏红花酸,经HPLC检测纯度达到98.43%,得率为8.42%。     

Quantitative analysis of major dibenzocyclooctane lignans in Schisandrae fructus by online TLC-DART-MS

Introduction – Direct analysis in real time (DART) ion source is a powerful ionising technique for the quick and easy detection of various organic molecules without any sample preparation steps, but the lack of quantitation capacity limits its extensive use in the field of phytochemical analysis. Objective – To improvise a new system which utilize DART‐MS as a hyphenated detector for quantitation. Methodology – A total extract of Schisandra chinensis fruit was analyzed on a TLC plate and three major lignan compounds were quantitated by three different methods of UV densitometry, TLC‐DART‐MS and HPLC‐UV to compare the efficiency of each method. To introduce the TLC plate into the DART ion source at a constant velocity, a syringe pump was employed. The DART‐MS total ion current chromatogram was recorded for the entire TLC plate. The concentration of each lignan compound was calculated from the calibration curve established with standard compound. Results – Gomisin A, gomisin N and schisandrin were well separated on a silica‐coated TLC plate and the specific ion current chromatograms were successfully acquired from the TLC‐DART‐MS system. The TLC‐DART‐MS system for the quantitation of natural products showed better linearity and specificity than TLC densitometry, and consumed less time and solvent than conventional HPLC method. Conclusion – A hyphenated system for the quantitation of phytochemicals from crude herbal drugs was successfully established. This system was shown to have a powerful analytical capacity for the prompt and efficient quantitation of natural products from crude drugs. Copyright © 2010 John Wiley & Sons, Ltd.     

桂黄降脂颗粒质量标准研究

目的:建立桂黄降脂颗粒的质量标准。方法:采用薄层色谱法对桂黄降脂颗粒中山楂、丹参进行定性鉴别;采用HPLC法对山楂中的槲皮素和丹参中的丹参素钠进行含量测定。结果:薄层色谱斑点清晰、分离度效果较好、且阴性无干扰;槲皮素在11.2~33.6μg范围内呈良好的线性关系,r=0.9995(n=5),样品平均回收率为98.00%,RSD 1.33%;丹参素钠在0.0166~0.332 mg·mL-1范围内呈良好的线性关系,r=0.9998(n=5),样品平均回收率为97.87%,RSD 1.35%。结论:该方法准确可靠、专属性强、重现性好,可以作为控制桂黄降脂颗粒质量的有效方法。     

A comprehensive study of eco-friendly natural pigment and its applications

Actinomycetes, a large group of filamentous bacteria account for 70–80% of secondary metabolites available commercially. The present investigation was undertaken with an aim to identify and characterize pigment from actinomycetes. Actinomycetes were isolated from rhizosphere soil samples collected from different regions of Madhya Pradesh state. Out of 85 actinomycetes, only 5 actinomycetes showed pigment production and based on diffusible pigment production ability one actinomycete ARITM02 was selected. The extraction of pigment was done by solvent extraction method using methanol and purified by TLC and column chromatography. The pigment was characterized by UV–Vis spectroscopy which showed the lamda maximum of 277.44. FTIR spectroscopy suggested various functional groups like amino group, amide group, hydroxide, benzene and lactone group. The Mass spectroscopy and NMR spectroscopy showed that the molecular mass of pigment is 621.7 and molecular formula is C34H43N3O8. The pigment was also tested for Antimicrobial activity against broad spectrum human pathogens, antioxidant test and toxicity test for safe use as a natural colorant in cosmetic, food, pharmaceutical and textile industries. The conclusion of study suggested that this novel pigment could be a versatile natural, safe and multipurpose.     

注射用红花黄色素辅助治疗早期糖尿病肾病的临床效果观察

目的：观察注射用红花黄色素辅助治疗早期糖尿病肾病（diabetic nephropathy,DN）的临床效果。方法：选择2011年10月至2012年2月我院收治的早期DN患者86例,在患者知情同意的情况下随机分为对照组（n=42例）和观察组（n=44例）,对照组采取西医常规治疗措施,观察组在上述治疗措施的基础上加用注射用红花黄色素治疗,治疗4周后,比较两组患者的实验室检查指标及临床疗效。结果：治疗4周后,观察组患者的白蛋白排泄率（UAER）、尿β2微球蛋白（β2-MG）、血肌酐（Scr）、血尿素氮（BUN）、血甘油三酯（TG）、血胆固醇（TC）、低密度脂蛋白（LDL）均显著低于对照组,差异均具有统计学意义（P〈0.05）;对照组治疗总有效率为85.7%,观察组治疗总有效率为97.7%,两组患者治疗总有效率比较,差异具有统计学意义（P〈0.05）,观察组优于对照组。结论：注射用红花黄色素治疗辅助治疗早期DN可有效其提高临床疗效。     

Synthesis, chromatographic purification, and analysis of isomers of biliverdin IX and bilirubin IX.

Neutral solvent systems were developed to isolate the alpha, beta, gamma, and delta isomers of biliverdin IX dimethyl ester by TLC. The individual free acids of biliverdin IX were obtained by saponification of the corresponding dimethyl esters. The bilirubin IX isomers were prepared by reducing the corresponding biliverdin IX isomers with NaBH3CN. Starting from a pure biliverdin IX dimethyl ester, the corresponding free acid of biliverdin IX or bilirubin IX was available within 3-4 h. Preparation of spectrally pure bile pigment required final TLC on acid-cleaned neutral TLC plates. The absorption spectra of the free acids and dimethyl esters of biliverdin IX in methanol showed a broad band at about 650 nm and a sharp band at about 375 nm. The long-wave-length band was extremely sensitive to the presence of strong acid. A 10-fold molar excess of HCl caused a 35- to 50-nm shift of the absorption maximum to longer wavelengths and near doubling of the maximum absorption. The molar absorption coefficients of biliverdins were identical for each free acid and dimethyl ester pair. In each case, Beer's law was followed in both methanol and acidified methanol. Methanol also proved to be a suitable solvent for spectroscopic determination of the non-alpha isomers of bilirubin IX. The wavelength of maximum absorption and molar absorption coefficient of each dipyrrolic ethyl anthranilate azo pigment derived from the various bilirubin IX isomers are also reported.     

从薄层层析到天然产物工业制备层析的理论与实践

基于分离理论的共性,通过薄层层析优化难分离物质对的最佳分离条件并直接放大到植物天然产物的工业制备分离。本文对实际应用中的溶剂组成、溶剂强度、溶剂用量及溶剂再利用等问题作了详细论述。最佳溶剂选择性可通过不同溶剂系统在薄层板上所给难分离物质对的最大Rf比值确定;在正相硅胶层析中,主要极性溶剂决定了物质的洗脱顺序;洗脱剂中极少量强极性溶剂(O．5％)或pH值的改变可显著改善拖尾现象;根据Rf值和容量因子(K)及洗脱体积三者之间的关系,Rf在0．1～0．3为用于柱层析的洗脱溶剂强度的最佳范围。     

Characterization and antifungal activity of the yellow pigment produced by a Bacillus sp. DBS4 isolated from the lichen Dirinaria agealita

This study emphasis the production of yellow pigment from endolichenic Bacillus sp. isolated from the lichen Dirinaria aegialita (Afzel. ex Ach.) B.J. Moore. Yellow pigment-producing twenty different strains were investigated. The hyperactive pigment-producing bacterial strain was identified as Bacillus gibsonii based on 99 % sequence similarity. Maximum bacterial pigment production appeared in Luria Bertani medium. Methanol extraction of the pigment and its partial purification using TLC was carried out. Furthermore, isolated pigments were characterized using UV-visible spectroscopy, FTIR spectroscopy, and GC-MS results related to the possibility of the carotenoid occurrence. The pigment also exhibited efficient antifungal activity against selected fungal pathogens of economic importance. Likewise, the pigment extract evaluated for the total antioxidant potential using Phosphomolybdenum and Ferric reducing antioxidant power assay and the results represented in Ascorbic Acid Equivalent (AAE)- 21.45 ± 1.212 mg/mL. The SC₅₀ of the pigment extract found to be 75.125 ± 0.18 µg/ml determined by the ABTS assay.     

小鼠脑组织中溶血卵磷脂和卵磷脂含量的简便分析方法

目的建立快速准确测定小鼠脑组织中卵磷脂（PC）和溶血卵磷脂（LPC）含量的简便方法。方法小鼠脑组织经氯仿和甲醇抽提总脂后,以氯仿/甲醇/乙酸/丙酮/水（40/25/7/4/2,v/v）为展层剂,采用单相薄层层析（TLC）并结合钼蓝定磷法测定两种磷脂的含量。结果该法测定PC和LPC的回收率分别为94.91%±6.74%和104.00%±5.38%,相对标准偏差分别为5.05%和7.10%,最低检测限为4.80nmol。用此法测得小鼠脑组织中PC和LPC的含量分别为20257.14±1022.88nmol/g脑重、420.91±29.87nmol/g脑重。结论TLC法用于小鼠脑组织中LPC等磷脂的测定,简便易操作、重现性好,不仅能够分离测定PC和LPC,而且能够分离测定小鼠脑组织中的另外其它5种磷脂。     

北青龙衣质量控制的研究

目的:建立北青龙衣质量控制的方法。方法:采用薄层色谱进行鉴别,展开条件为三氯甲烷-甲醇(8:2),采用高效液相色谱进行含量测定,以乙腈-水-磷酸(10:90:0.2)为流动相,指标成分为(4S)-4,5-二羟基-α-四氢萘酮-4-O-β-D-吡喃葡糖苷。结果:方法灵敏、可靠、准确、重复性好。结论:该方法可作为北青龙衣质量控制的方法。