Preparation Process and Thin Layer Chromatography Identification of Wufang Babu Poultice

[Objectives] To establish the process flow of preparation of Wufang Babu Poultice and the identification method of thin layer chromatography (TLC). [Methods] For the forming process of Wufang Babu Poultice, the preparation method of mixed pharmaceutical powder with suitable pharmaceutical excipients was adopted. Qualitative identification of medicinal materials in Wufang Babu Poultice (Strychni Semen, Rhei Radix Et Rhizoma, Dipsaci Radix, and Angelicae Sinensis Radix) was carried out by TLC. [Results] Mixed pharmaceutical powder mixed with glycerol, gelatin and other pharmaceutical excipients can be prepared for forming. The test solution chromatography of each medicinal material (Strychni Semen, Rhei Radix et Rhizoma, Dipsaci Radix, Angelicae Sinensis Radix) showed pigment spots of the same color at the same position as its corresponding control medicinal materials and reference chromatography, and the display was clear. [Conclusions] The preparation process is simple and feasible, and can be used as the forming process of Wufang Babu Poultice. The TLC determination method is simple to operate, has good specificity, and has no effect on negative results, and can be used for identification of Wufang Babu Poultice.

Comparison of liquid-liquid extraction-thin layer chromatography with solid-phase extraction-high-performance thin layer chromatography in detection of urinary morphine

Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.

Secondary metabolite credentials ofEvolvulus alsinoides by high performance thin layer chromatography(HPTLC)

Plants and plant-based products are the bases of many modern pharmaceuticals that are current in use today for various diseases.The aim of the study was to investigate the biochemical constituents and high performance thin layer chromatography（HPTLC） finger printing of the ethanolic extract of Evolvulus alsinoides.Phytochemical screening was done by standard procedures and HPTLC method was also established to analyze alkaloids,flavonoids and phenolic compounds from the ethanolic extract of Evolvulus alsinoides.Preliminary phytochemical screening showed that ethanol extracted more secondary metabolites than other solvents.HPTLC fingerprinting analysis showed the presence of various alkaloids,flavonoids and phenols（quercetin） in the ethanolic extract.It can be concluded that Evolvulus alsinoides may serve as a source of potent antioxidants that may be used in the prevention of various diseases such as cancer,diabetes and cardiovascular diseases due to the presence of phenolic compounds.HPTLC finger print of Evolvulus alsinoides may be useful in the differentiation of the species from adulterants and act as a biochemical marker for this medicinally important plant in the pharmaceutical industry and plant systematic studies.

Evaluation of quantitative variation of secondary metabolites in Bergenia ciliata(Haw.)using high performance thin layer chromatography

Dear Editor： Therapeutically active metabolite contents in a med- icinal plant vary in nature, which may impact on its therapeutic efficacy. Bergenia （Saxifragaceae） is an evergreen perennial herb widely distributed in Central and East Asia with about 30 species reported worldwide. It grows at a range of altitudes from the Khasia hills at 400 feet to the temperate Himalayas from Kashmir to Bhutan at 7,000-10,000 feet. Its distribution over a wide range of altitudinal zones makes it a good candidate for studying variations in its metabolic profiles under different climatic conditions. Bergenin （C-glycoside of 4-O-methyl gallic acid） has been identified as a potent active secondary metabolite in Bergenia and other therapeutically active constituents including, among others, gallic acid （3,4,5 trihydroxybenzoic acid）, （＋） catechin, and gallicin （Fig. 1）.

Application of Thin Layer Chromatography in Preparation of Drug Containing Serum of Eucalyptus Oil

[Objectives] To explore whether the thin layer chromatography( TLC) can be used to guide the preparation of drug containing serum of eucalyptus oil. [Methods]Eucalyptus oil samples with different dilution ratio were detected by TLC. Eucalyptus oil was intragastrically administered to mice,serum samples of different eucalyptus oil doses,different intragastric administration methods and different blood sampling times were collected. The above samples were detected by TLC,and the above results were verified by gas chromatography. [Results] TLC can detect concentration difference of eucalyptus oil samples with different dilution ratio. TLC can provide qualitative and semi-quantitative detection of eucalyptus oil in serum. High,medium and low dose of eucalyptus oil in serum had different effects on the growth of MCF-7 cells in the SD rats( P < 0. 05). [Conclusions] TLC can be used to guide the preparation of drug containing serum of eucalyptus oil.

Identification of Ethnic Medicine Polygonum capitatum by Thin Layer Chromatography

[Objectives]To establish a thin-layer chromatography identification method for the ethnic medicinal materials of Polygonum capitatum.[Methods]The thin layer chromatography(TLC)method was used to identify materials.[Results]The TLC identification showed that in the chromatogram of the test sample,there were spots of the same color in the corresponding position of the chromatogram of the reference medicinal material,and the reproducibility was good.[Conclusions]The TLC identification and the determination results of the inspection items can provide a basis for the quality control of the medicinal materials of P.capitatum.

DETERMINING THE CONTENT OF JASMINODIN IN MEI RONG CAPSULE WITH THIN LAYER CHROMATOGRAPHY

Objective Jasminodin in Mei Rong capsule was determined by the method or thin layer chromatog- raphy. Mothods The sample Jasminodin was extracted with methanol and then the extract was chromatographed on silica gel GF254 plate with chloroform-methanol-water(10:3:1) as mobile phase and the chromatograms were scanned by using Shimadzu CS-930 dual wavelength TLCS in zegzag scanning mode at λ_s 370nm and λR 250nm. Results Callbration graph was rectilinear between 2.7μg^16.2μg per spot for the jasminodin. Conclusion Satisfa- tory results were obtained with the average recovery ratio of 99.76%,RSD 2.27%.

Thin layer chromatography performed in stages to identify the presence of aromatic like fraction in chosen bitumen modifiers

The organic modifiers are used to alter the rheology of the binder in the asphalt concrete at an added cost. For quality control purpose, recognizing if such material is present in the final blend is of an interest. The thin layer chromatography(TLC) using a flame photometric detector(FPD), in addition to the typical flame ionization detector, was demonstrated hereby as a potential analytical tool for this problem, differentiating between tall crude oil based anti-aging agent, polymer, oxidized bitumen and gilsonite. Gilsonite and anti-aging agent consists of the material soluble in solvent used in the development of the fraction referred to as aromatics. Due to the hindered mobility of modifier molecules on the stationary phase, the elution of aromatic fraction stops at position convoluted with polars I and polars II fraction regions, colloquially referred to as resins and asphaltenes. However,for the color of this fraction within gilsonite is different. The presence of gilsonite is thus identifiable visually after the second development bath, but also to an extent with FPD from the final chromatogram. The thin layer chromatography-flame ionization detectors(TLC-FID) procedure is suggested to be supplemented by infrared spectroscopy to discriminate between non-bituminous and bituminous modifiers of similar response during fractionation.

Separation and Detection of Ceramides by HPLC Followed by Evaporative Light-Scattering Detection and Thin Layer Chromatography

Ceramides are important signaling molecules involved in a variety of cellular processes, including cell growth, differentiation, and apoptosis. Currently, different methods are used for ceramide analysis, some of which are insensitive or cumbersome. This paper described methods utilizing thin layer chromatography (TLC) and high-performance liquid chromatography (HPLC) followed by evaporative light scattering detection (ELSD) to detect ceramide directly in cell extracts without derivatization, which was proved to be efficient and reproducible. Five kinds of ceramides were used as standards. Both TLC and normal-phase HPLC/ELSD results indicate that yeast contains several kinds of ceramides.

Algerian mint species:high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

Objective:To determine the quantitative paremeters of rosmarinic acid in Algerian mints,Mentha spicata L.(M.spicata),Mentha pulegium L.and Mentha rotundifolia(L.)Huds by high performance thin layer chromatography(HPTLC)-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation.Methods:The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform:acetone:formic acid(75:16.5:8.5,v/v)as the mobile phase.Rosmarinic acid was determined in UV at 365 nm and fluorescence at λ_(exc)325 nm with a 550 nm filter,respectively.The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method.Results:Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1000 ng/spot.M.spicata was found to contain significantly higher concentrations of rosmarinic acid.The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision(total precision for Mentha spp extracts,5.1%and 5.8%for UV and fluorescence detection,respectively).The HPTLC data,allied to assays of linoleic acid peroxidation prevention,suggested the potential of M.spicata(52%Trolox®equivalents)as a natural source for inhibitors of lipid peroxidation.Conclusions:Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

Identification of Xunxi Shujin Decoction by TLC

[Objectives]To establish a TLC qualitative method for the determination of Radix Aconiti,Radix Aconiti Kusnezoffii,Caesalpinia sappan L.and Radix zanthoxyli.[Methods]TLC was used to study the quality of Radix Aconiti,Radix Aconiti Kusnezoffii and C.sappan L.in Xunxi Shujin Decoction,and the influencing factors were investigated to optimize the TLC conditions.[Results]In the TLC identification test of Radix Aconiti,Radix Aconiti Kusnezoffii,C.sappan L.and R.zanthoxyli in Xunxi Shujin Decoction,the spots were clear,the resolution was good,the specific value was moderate,the negative control was not disturbed,and the specificity was strong.[Conclusions]The established TLC method was simple,specific and reproducible,and could be used for the quality control of Xunxi Shujin Decoction.

Study on Quality Standards of Jianjin Zhuanggu Paste

[Objectives]Some Chinese medicinal materials of Jianjin Zhuanggu Paste were microscopically identified,and several active ingredients were studied by thin-layer identification,which provides reference for further improving the quality standards of hospital preparations.[Methods]The effective components of Jianjin Zhuanggu Paste were qualitatively identified by thin-layer chromatography(TLC).[Results]The microscopic identification of the three Chinese medicinal materials in Jianjin Zhuanggu Paste showed the microscopic characteristics of Radix Codonopsis,Radix Astragali and Radix Notoginseng.TLC identification showed that there were characteristic spots of Radix Codonopsis,Radix Astragali,Radix Rehmanniae Preparata and Radix Notoginseng in Jianjin Zhuanggu Paste.[Conclusions]This study established the quality standard research method of Jianjin Zhuanggu Paste,which further strengthens the safety standards of hospital preparations,and improves the clinical efficacy of drugs,as well as the quality standards of hospital preparations to a certain extent.

Quality Standard of Oxyria sinensis Hemsl

[Objectives]To establish the quality standard of Oxyria sinensis Hemsl.[Methods]The method in Chinese Pharmacopoeia(2020 edition)was used to determine the moisture,total ash,acid-insoluble ash and alcohol-soluble extracts of O.sinensis.The qualitative identification of medicinal materials was carried out by microscopic identification method and thin layer chromatography(TLC).The contents of hyperoside and isoquercitrin were determined by high performance liquid chromatography(HPLC).[Results]The total amount of moisture,total ash,acid-insoluble ash,alcohol-soluble extract,hyperoside and isoquercitrin of 12 batches of medicinal materials were 8.56%-11.53%,11.26%-15.48%,1.62%-2.56%,17.75%-26.09%,and 0.036%-0.42%,respectively.The microscopic features were obvious,and pores,fibers,calcium oxalate clusters,calcium oxalate square crystals,cork cells could be observed.Fluorescent spots of the same color were displayed at the positions corresponding to the hyperoside reference substance.[Conclusions]Establishing relatively complete quality standards for O.sinensis medicinal materials can provide a reference for the quality control of medicinal materials.

Quality Control of Zhuang Medicine Xiaoyan Zhiyang Lotion

[Objectives]To establish the TLC identification methods of Llicis Rotundae Cortex and Mahoniae Caulis and the determination method of syringin content in Zhuang Medicine Xiaoyan Zhiyang Lotion.[Methods]Thin layer chromatography(TLC)was used to qualitatively identify Llicis Rotundae Cortex and Mahoniae Caulis in Zhuang Medicine Xiaoyan Zhiyang Lotion.The quantitative analysis of syringin in Zhuang Medicine Xiaoyan Zhiyang Lotion was carried out by high-performance liquid chromatography(HPLC).Chromatographic conditions are as follows:Luna 5μm C_(18)((2)100 A(250 mm×4.6 mm,5μm)column was adopted;acetonitrile(10%)-water(90%)was as the mobile phase,and the flow rate was 1.0 mL/min;the detection wavelength was 265 nm;the sample size was 5μL;the column temperature was 30℃.[Results]Syringin had a good linear relationship with its peak area in the range of 0.190-2.856μg(R^(2)=0.9995).The RSD values of precision,stability and repeatability experiments were all lower than 2.5%,and the average sampling recovery rate(n=6)was 100.37%(RSD=-0.88%).[Conclusions]The method had the advantages of simple operation,strong specificity,good repeatability and stability,and can be used for the quality control of Zhuang Medicine Xiaoyan Zhiyang Lotion.

浸渍硅胶薄层色谱板分离钴和镍及数字图像分析法定量(英文)

Thin layer chromatography(TLC) of cobalt and nickel has been performed on silica gel layers induced with alkali mediated cellulose extract.A novel combination of 10% aqueous solutions of Tween-20 and potassium thiocyanate in 1∶1(v/v) was identified as the best mobile phase for the selective separation of Co2+from Ni2+on the impregnated Silica Gel G layers.The chromatographic characteristics of the cations were studied and the limits of detection as well as the limits of quantification for Co2+and Ni2+were determined.The quantitative estimation of the cations was achieved from the digital image analysis of respective chromatograms.The proposed quantitative method was successfully applied with 0-0.50% error for the determination of Co2+from Ni2+in spiked samples of bauxite,soil and rock containing common cations such as Al3+,Fe2+,Ti4+,Zn2+,Mn2+,Cu2+,Cr6+,Mg2+,etc.under the optimized chromatographic conditions.

Bioautography and its scope in the field of natural product chemistry

Medicinal plants, vegetables and fruits are the sources of huge number of bioactive lead/scaffolds with therapeutic and nutraceutical importance. Bioautography is a means of target-directed isolation of active molecules on chromatogram. Organic solvents employed in chromatographic separation process can be completely removed before biological detection because these solvents cause inactivation of enzymes and/or death of living organisms. They offer a rapid and easy identification of bioactive lead/scaffolds in complex matrices of plant extracts. Bioautography is a technique to isolate hit（s）/lead（s） by employing a suitable chromatographic process followed by a biological detection system. This review critically describes the methodologies to identify antimicrobial, antioxidant, enzyme inhibitor lead/scaffolds by employing bioautography. A significant number of examples have been incorporated to authenticate the methodologies.

Studies on Determining Method of Trehalose

Trehalose can be determined by thin layer chromatography and high performance liquid chromatography. But it's difficult to distinguish trehalose from the similar bisaccharides. If the reaction of the reduced bisaccharides with phenyl hydrazine to form osazone is used, then the disturbance of the similar reduced bisaccharides can be rapidly and conveniently excluded, or via the ammoniated-reduced reaction, aliline can be specially bounded to the reduced hydroxyl of the bisaccharides. In that way trehalose can be accurately determined.

Enhancement of Urinary Elimination of 3-Bromobenzanthrone Metabolites by Oral Supplementation of Ascorbic Acid in Guinea Pigs

Objective 3-Bromobenzanthrone (3-BBA), an anthraquinone intermediate dye, is extensively used in textile industry. Since, our prior studies have shown that 3-BBA caused significant depletion of ascorbic acid (AsA) levels, the effect of exogenous supplementation of AsA on the urinary elimination of 3-BBA metabolites was investigated. Method Guinea pigs were treated with single oral dose of 3-BBA (50 mg/kg b. wt.) in groundnut oil while another group was treated with single oral dose of 3-BBA (50 mg/kg b. wt.) along with 3 day prior and post oral supplementation of AsA. Control groups were either treated with groundnut oil or AsA alone. Urine from individual animals was collected, extracted and analysed on HPTLC. Results The highest elimination of 3-BBA (75 mg) was found to be in 0-24 h urine fraction which decreased to 18 mg and 5 mg in the two subsequent 24 hourly fractions of urine. Exogenous supplementation of AsA increased the total urinary elimination of 3-BBA by almost 77%. A total of 10 fluorescent metabolites excluding the parent compound were eliminated in the urine of guinea pigs treated with 3-BBA. Densitometric scanning of chromatogram showed different peaks at Rf 0.18, 0.22, 0.27, 0.34, 0.40, 0.48, 0.56, 0.66, 0.72, 0.80, and 0.95 which were eliminated and marked as urinary metabolite 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, and 11 respectively. AsA not only significantly enhanced the elimination of 3-BBA metabolites but also modified the pattern of metabolites drastically in 0-6 h, 6-24 h and 24-48 h urine fractions. Conclusion These results indicate that AsA may be useful in protecting the toxicity of 3-BBA by fascilitating the urinary metabolite(s) excretion of 3-BBA.

磷酸钛离子交换薄层色谱分离无机离子(英文)

The chromatographic behavior of 30 inorganic cations has been studied on thin layers of titanium phosphate ion-exchanger using several aqueous,organic and mixed mobile phases.The separation of one ion from several other ions and also ternary and binary separations have been developed.Some important analytical separations are reported.The effect of pH of the mobile phase on retention factor(Rf)values of the cations in the presence of complex-forming anion along with the separation power of the ion-exchanger were studied.This ion-exchanger exhibits high sorption capacity and varying selectivity towards metal ions and makes it a suitable stationary phase in thin layer chromatography.

异丙肾上腺素在硅酸铋离子交换薄层上的选择性分离与测定（英文）

A simple and sensitive method for the separation and determination of isoproterenol from other doping drugs has been developed on thin layers of bismuth silicate,a synthetic inorganic ion exchanger as adsorbent in thin layer chromatography(TLC).A mixture of methanol and 0.1 mol/L formic acid(3∶7,v/v)was employed as the mobile phase.The development time was 32 min.The quantitative measurement were performed with a Camag TLC Scanner-3 at wavelength(λ)of 410 nm.The isoproterenol recovery in this procedure was 98.9%.The linear correlation coefficient was greater than 0.987 1 and the relative standard deviation(RSD)was less than 0.94.The limit of detection(LOD)and limit of quantification(LOQ)were 7.7×10-7mol/L and 3.85×10-6mol/L,respectively.This method has been applied in the determination of isoproterenol in dosage forms and in biological fluids.