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ObjectiveTo establish the identification method of Dalbergiae Odoriferae Lignum（DOL） and its counterfeits by nuclear magnetic resonance hydrogen spectrum（1H-NMR） combined with multivariate statistical analysis. Method1H-NMR spectra of DOL and its counterfeits were obtained by NMR， and the full composition information was established and transformed into a data matrix， and the detection conditions were as follows：taking dimethyl sulfoxide-d6（DMSO-d6） containing 0.03% tetramethylsilane（TMS） as the solvent， the constant temperature at 298 K（1 K=-272.15 ℃）， pulse interval of 1.00 s， spectrum width of 12 019.23 Hz， the scanning number of 16 times， and the sampling time of 1.08 s. Similarity examination and hierarchical cluster analysis（HCA） were performed on the data matrix of DOL and its counterfeits， and orthogonal partial least squares-discriminant analysis（OPLS-DA） was used to analyze the data matrix and identify the differential components between them. In the established OPLS-DA category variable value model， the category variable value of DOL was set as 1， and the category variable value of the counterfeits was set as 0， and the threshold was set as ±0.3， in order to identify the commercially available DOL. The OPLS-DA score plot was used to determine the types of counterfeits in commercially available DOL， and it was verified by thin layer chromatography（TLC）. ResultThe results of similarity analysis and HCA showed that there was a significant difference between DOL and its counterfeits. OPLS-DA found that the differential component between DOL and its counterfeits was trans-nerolidol. The established category variable value model could successfully identify the authenticity of the commercially available DOL. The results of the OPLS-DA score plot showed that there were heartwood of Dalbergia pinnata and D. cochinchinensis in the commercially available DOL， and were consistent with the TLC verification results. ConclusionThere is a phenomenon that heartwood of D. pinnata and D. cochinchinensis are sold as DOL in the market. 1H-NMR combined with multivariate statistical analysis can effectively distinguish DOL and its counterfeits， which can provide a reference for the identification of them.
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ObjectiveTo establish the specific chromatogram and thin layer chromatography（TLC） identification method of Kaixinsan（KXS） samples， in order to clarify the key quality attributes and provide reference for the quality evaluation of KXS. MethodHigh performance liquid chromatography（HPLC） specific chromatogram of KXS was developed with YMC Hydrosphere C18 column（4.6 mm×250 mm， 5 μm）， the mobile phase was acetonitrile（A）-0.2% formic acid aqueous solution（B） for gradient elution（0-15 min， 2%-20%A； 15-25 min， 20%-25%A； 25-30 min， 25%-30%A； 30-45 min， 30%-31%A； 45-50 min， 31%-44%A； 50-65 min， 44%-45%A； 65-73 min， 45%-75%A； 73-95 min， 75%-100%A； 95-105 min， 100%A； 105-105.1 min， 100%-2%A； 105.1-120 min， 2%A）， the detection wavelength was 320 nm. Ultra high performance liquid chromatography-linear ion trap-electrostatic field orbitrap mass spectrometry（UHPLC-LTQ-Orbitrap MS） was used to identify the chemical components of KXS with electrospray ionization（ESI）， negative ion mode and scanning range of m/z 50-2 000. TLC identification methods for Poria and Ginseng Radix et Rhizoma in KXS were established. ResultThere were 11 common peaks in the specific chromatogram of KXS， attributed to Polygalae Radix， Poria and Acori Tatarinowii Rhizoma. Taking peak 9（α-asarone） as the reference peak， the relative standard deviations of the retention times of 15 batches of KXS samples were<0.2%. A total of 34 compounds were identified by UHPLC-LTQ-Orbitrap MS， including terpenoids， phenylpropanoids， oligosaccharides and ketones. The established TLC had good separation and was rapid， reliable， simple， feasible， suitable for the identification of Poria and Ginseng Radix et Rhizoma in KXS. ConclusionThe specific chromatogram and TLC of KXS are stable and reproducible. The material basis of KXS is basically clarified by MS， which can provide a reference for the development and quality control of KXS.
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ObjectiveTo establish the specific chromatogram and thin layer chromatography（TLC） of Qingxin Lianziyin（QXLZY） benchmark samples， in order to clarify the key quality attributes and provide a reference for the quality evaluation of QXLZY. MethodHigh performance liquid chromatography（HPLC） specific chromatogram of QXLZY benchmark samples was developed by using a YMC Hydrosphere C18 column（4.6 mm×250 mm， 5 μm） with the mobile phase of acetonitrile（A）-0.2% formic acid aqueous solution（B） for gradient elution（0-10 min， 5%-20%A； 10-20 min， 20%A； 20-25 min， 20%-24%A； 25-40 min， 24%-30%A； 40-55 min， 30%-50%A； 55-65 min， 50%-100%A； 65-75 min， 100%A； 75-75.1 min， 100%-5%A； 75.1-90 min， 5%A）， and the detection wavelength was 360 nm. Ultra-high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry（UHPLC-LTQ-Orbitrap MS） with electrospray ionization（ESI） was used to identify the components of QXLZY benchmark samples by accurate relative molecular weight and multilevel MS fragment ion information， the detection conditions were positive and negative ion modes and data dependency scanning mode. TLC identification methods for Ophiopogonis Radix， Lycii Cortex， Nelumbinis Semen， Poria， Astragali Radix and Ginseng Radix et Rhizoma in QXLZY were established. ResultA total of 15 characteristic peaks were identified from Glycyrrhizae Radix et Rhizoma， Plantaginis Semen and Scutellariae Radix， and the relative standard deviations of the retention times of 15 characteristic peaks in 15 batches of QXLZY benchmark samples were≤3% with peak 8（baicalin） as the reference peak. A total of 100 compounds， including flavonoids， organic acids， saponins， amino acids and others， were identified in the benchmark samples by UHPLC-LTQ-Orbitrap MS. The established TLC had good separation and was suitable for the identification of Ophiopogonis Radix， Lycii Cortex， Nelumbinis Semen， Poria， Astragali Radix and Ginseng Radix et Rhizoma in QXLZY. ConclusionThe material basis of QXLZY benchmark samples is basically determined by MS designation and source attribution. The established specific chromatogram and TLC of QXLZY are simple， stable and reproducible， which can provide a reference for the development and quality control of QXLZY.
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ObjectiveTo investigate the quality of Amomi Fructus in the market， and to compare the difference between the seed mass and shell， so as to provide a basis for standardizing the usage of Amomi Fructus. MethodThe properties， thin layer identification， moisture， the content of bornyl acetate were determined by the methods in the 2020 edition of Chinese Pharmacopoeia， and the ash and extract content were determined according to the collection method of the 2020 edition of Chinese Pharmacopoeia. ResultAmong the 17 batches of samples， except the content of bornyl acetate in 2 batches of Amomum longiligulare， 2 batches of A. longiligulare and A. villosum mixture was lower than the standard， the quality of other samples all met the standard of the 2020 edition of Chinese Pharmacopoeia， but there were two specifications with shell and without shell. The husk rate， volatile oil， extract and bornyl acetate contents of the seed mass and shell were tested. It was found that the content of volatile oil in three kinds of Amomi Fructus seed mass was 1.8-5.3 times that of the corresponding shell， and the content of bornyl acetate in the seed mass was 8.8-62.1 times that of the corresponding shell， but there was little difference in the extract content. ConclusionBased on the above research， it is considered that the content of bornyl acetate in A. longiligulare contained in the 2020 edition of Chinese Pharmacopoeia remains to be discussed. It is tentatively determined that the total ash content of Amomi Fructus should not be more than 10.0%， and the extract content should not be less than 15.0%. At the same time， it is suggested that when Amomi Fructus is used as medicine， the dosage of Amomi Fructus should be calculated according to the removal rate of 20%-30% of shell， and it should be crushed regardless of whether it is used in shell or not.
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ObjectiveTo improve the current standard of Belladonnae Herba in the 2020 edition of Chinese Pharmacopoeia. MethodTaking hyoscyamine sulfate， atropine sulfate and scopoletin as reference substances， and ethyl acetate-methanol-concentrated ammonia（17∶4∶2）as developing solvent， thin layer chromatography （TLC） was applied in the qualitative identification of Belladonnae Herba. The moisture， total ash and ethanol-soluble extract of Belladonnae Herba were determined based on the general principles in the 2020 edition of Chinese Pharmacopoeia （volume Ⅳ）. The contents of hyoscyamine sulfate and scopolamine hydrobromide were analyzed by high performance liquid chromatography （HPLC） with mobile phase of acetonitrile-54 mmol·L-1 phosphate buffer solution （14∶86）， flow rate of 1.0 mL·min-1 and detection wavelength at 210 nm. ResultThe spots in the TLC were clear with good separation and specificity. Hyoscyamine sulfate and scopolamine hydrobromide showed a good linearity with peak area in the range of 0.024 7-0.789 6 g·L-1 （r=0.999 9） and 0.003 9-0.124 0 g·L-1 （r=0.999 9）， the average recoveries of these two ingredients were 100.29% （RSD 1.6%） and 99.04% （RSD 1.4%）， respectively. The limits for moisture， total ash in Belladonnae Herba should be less than 13.0% and the limit for the ethanol-soluble extract should be more than 10.0%. Due to the low content and wide variation of scopolamine hydrobromide， the content of hyoscyamine sulfate should not be less than 0.098%. ConclusionThe established method is simple， specific and reproducible， which can be used to improve the quality control standard of Belladonnae Herba.
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ObjectiveTo establish the quality standard of Liangditang benchmark samples. MethodUltra performance liquid chromatography-quadrupole time-of-flight mass spectrometry （UPLC-QTOF-MS） was used to qualitatively analyze the chemical composition of Liangditang on the basis of molecular and fragment ion peak information with cracking law. The mobile phase was methanol （A）-0.05% phosphate aqueous solution （B） for gradient elution （0-10 min， 5%-23.5%A； 10-20 min， 23.5%A； 20-58 min， 23.5%-63%A； 58-60 min， 63%-90%A）， the flow rate was 0.8 mL·min-1， and the detection wavelength was 254 nm. Electrospray ionization was employed under positive ion mode， the detection range was m/z 100-1 700. Key quality attributes and sources were determined by comparing with single medicine and reference substances. Through mass transfer analysis of multiple batches from decoction pieces to benchmark samples， high performance liquid chromatography （HPLC） for determining the contents of index components and HPLC detection of characteristic maps were established. Through the determination of 15 batches of benchmark samples， the content range of the index components and the common peaks of the characteristic map were determined. Thin layer chromatography （TLC） was applied to the identification of 5 medicines in the formula. Moisture and dry extract yield of the benchmark samples were determined by drying method. ResultA total of 27 compounds were inferred from the benchmark samples of Liangditang， among which 9 compounds were confirmed by comparison with the control， including catalpol， harpagide， gallic acid， albiflorin， paeoniflorin， verbascoside， angoroside C， cinnamic acid and harpagoside. A method for determining the characteristic maps of the benchmark samples were established and 13 peaks were assigned， and the characteristic peaks were mainly derived from wine-processed products of Rehmanniae Radix， Scrophulariae Radix and wine-processed products of Paeoniae Radix Alba. The similarity between the characteristic map of 15 batches of benchmark samples and the control characteristic map was >0.9. Methods for the determination of paeoniflorin， harpagoside， L-hydroxyproline and glycine were established， and the contents of these four components in 15 batches of benchmark samples were within ±30% of the corresponding mean value， and the transfer rate of decoction pieces to the benchmark samples was stable and controllable. TLC was established to identify 5 prescription drugs （except Ejiao） with two kinds of test solutions， and the results showed that the method had good specificity. The average dry extract yield was 48.06%， and the average moisture was 5.58%， which were within the range of ±10% and ±30% of their mean values， respectively. ConclusionThe quality standard of Liangditang benchmark samples was as follows：the similarity between the benchmark samples and the control characteristic map is >0.9， the contents of paeoniflorin， harpagoside， L-hydroxyproline and glycine are 217-403， 24-46， 634-1 178， 1 253-2 328 mg per dose， the dry extract yield is 43.0%-53.0%， the moisture is 4.0%-7.0%， under the set detection conditions， the benchmark samples have corresponding characteristic spots by comparing with the control herbs of 5 medicines. This quality standard is stable and reliable， which fills the gap in the quality control of Liangditang， and can provide a reference for the establishment of the quality standard of Liangditang granules.
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In view of the current inadequate standards for Gleditsiae Spina in the Chinese Pharmacopoeia, this study put forward some new items of the quality standards of Gleditsiae Spina. Thin-layer chromatography(TLC) was performed for identification with the reference substance of taxifolin and the reference material of Gleditsiae Spina as the control. According to the general principles of the Chinese Pharmacopoeia(2020 edition, Vol. 4), the moisture, total ash content, and alcohol-soluble extract of medicinal materials and decoction pieces of Gleditsiae Spina were determined. The content determination method for medicinal materials and decoction pieces of Gleditsiae Spina was established using high-performance liquid chromatography(HPLC), with taxifolin as the quality control index. Based on the determination results of 30 batches of samples of Gleditsiae Spina from different habitats, the draft quality standards of Gleditsiae Spina were developed, which provided suggestions for the revision of the quality standards of Gleditsiae Spina in the Chinese Pharmacopoeia.
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Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Quality Control , Reference StandardsABSTRACT
Objective:To establish a thin layer chromatography （TLC） identification method for different processed products of Rehmanniae Radix. Method:Catalpol， D-fructose， sucrose， raffinose， stachyose， melibiose and manninotriose were used as control substances， and the effects of extraction solvents （water， 20% methanol， 50% methanol， 80% methanol）， developing solvents （n-butanol-methanol-chloroform-glacial acetic acid-water， ethyl acetate-pyridine-glacial acetic acid-water， n-butanol-glacial acetic acid-water）， color reagents （aniline-diphenylamine-phosphoric acid solution， ninhydrin solution）， sampling volumes （2， 4， 6 μL） and inspection conditions （sunlight， bottom lamp of sunlight， 365 nm， 254 nm） on TLC were investigated to determine the preparation method of sample solution of Rehmanniae Radix and Rehmanniae Radix Praeparata and the optimal TLC conditions. Result:High performance silica gel G plate was used for TLC， n-butanol-methanol-chloroform-glacial acetic acid-water （13∶5∶5∶1∶2） was used as developing agent， aniline-diphenylamine-phosphoric acid solution was sprayed and heated at 110 ℃ for color development， and then inspected under the bottom lamp of sunlight. The separation and color development of different processed products of Rehmanniae Radix were good with clear spots and good characteristics. Conclusion:The established TLC is simple and easy to operate with obvious qualitative characteristics and intuitive results. It can effectively identify different processed products of Rehmanniae Radix and provide experimental basis for determining the end point of processing of Rehmanniae Radix Praeparata.
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Objective:There were 92 kinds of compound preparations containing Ophiopogonis Radix in the 2015 edition of Chinese Pharmacopoeia， but there was no effective method to identify these compound preparations. Because Ophiopogonis Radix and Liriopes Radix are similar in appearance， it is easy to be confused in application. The aim of this study was to set up a thin layer chromatography （TLC） to identify compound preparations containing Ophiopogonis Radix and distinguish Ophiopogonis Radix and Liriopes Radix in the forms of decoction pieces and standard decoction. Method:In this study， decoction pieces of Ophiopogonis Radix and Liriopes Radix were collected and separately prepared as standard decoction. TLC was used to qualitatively identify decoction pieces and standard decoction of Ophiopogonis Radix and Liriopes Radix， and compound preparations containing Ophiopogonis Radix. In the TLC， the lower solution of chloroform-methanol-water （65∶35∶10） was selected as the developing agent and 10% sulfuric acid ethanol solution as the chromogenic agent. Result:The resolution of this TLC was good. Decoction pieces， standard decoction and preparations of Ophiopogonis Radix had the same characteristic strips， which were two bright white fluorescent strips under ultraviolet lamp （365 nm）. But these two characteristic strips were not existed in the TLC of decoction pieces and standard decoction of Liriopes Radix. The corresponding components of both of these two strips were identified as mixture containing saponins by LC-MSn， including ophiopogonin Ra， Tb， ophiopogonin D'， borneol glycoside， ophiopogonin C and Liriope muscari baily saponins C. Conclusion:The established TLC method， which has significant advantages such as high specificity and sensitivity， can be applied to the characteristic identification of decoction pieces and standard decoction of Ophiopogonis Radix， the identification of compound preparations containing Ophiopogonis Radix， and the distinction of Ophiopogonis Radix and Liriopes Radix， thus serving as an effective method to qualitatively identify Ophiopogonis Radix and its compound preparations.
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Objective: To extract the volatile oil in Semen Ocimi Basilici(SOB),determine the chemical con- stituents of the volatile oil extract the polysaccharide from the SOB residue after extracting the volatile oil,and analyze the monosaccharide compositions of the polysaccharide. Methods: The SOB volatile oil was extracted by the simultane- ous distillation and extraction(SDE)method and by the conventional method of steam distillation,respectively,and the chemical constituents of the oils were analyzed and identified by the gas chromatography- mass spectrometry(GC- MS). Polysaccharides in the SOB residues were obtained by the water extraction,followed by the alcohol precipitation,and the monosaccharide compositions of the polysaccharide were analyzed by the thin layer chromatography (TLC). Results In total 51 compounds were identified in the SOB volatile oil extracted by the SDE method,accounting for 91.76% of the total oil amount,involving the alkanes,alkenes,alkynes,alcohols,esters,aldehydes,acids,ketones, ethers,acyl chloride,heterocycles,amide and other substances. In total 43 compounds were identified in the SOB vola- tile oil extracted by the conventional steam distillation,accounting for 88.20% of the total oil amount,which was related to the alkanes,alkenes,alkynes,alcohols,esters,aldehydes,acids,ethers,ketones,heterocycles,amides and other substances. The monosaccharide composition analysis showed that the SOB polysaccharide was composed of 5 kinds of monosaccharides. Conclusion: Among the identified compounds,only 9 compounds existed in the SOB volatile oils extracted by two different Methods:,indicating that the combined use of the two different extraction Methods: may be more powerful for comprehensive analysis of the chemical constituents of SOB volatile oil.
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ABSTRACT The aim of this study is the production, purification, and characterisation of thermostable raw starch hydrolyzing α-amylase produced by Bacillus mojavensis SO-10. The maximum production conditions of α-amylase were found at 36th hour, 35 °C and pH 7.0. We utilized three steps to purify the thermostable α-amylase and as a result, 34-fold and 18% yield were obtained. The molecular weight of purified α-amylase was determined as 73 kD. The Km and Vmax rates were detected as 0.010 mM and 3.38 µmol min−1, respectively. This purified α-amylase exhibited the highest activity at pH 5.0-6.0 and 70 ºC and showed stability over a wide variety of pH and temperature at 4.0-8.0, and 40-50 ºC, respectively. The thermostable purified α-amylase exhibited stability in the presence of denaturing agents and heavy metal ions. The purified enzyme hydrolyzed the raw starches of corn and wheat grains in the ratio of 36.7% and 39.2% respectively. The end-yields of soluble starch hydrolysis were analyzed by thin-layer chromatography (TLC). In addition, the usage of purified α-amylase in clarification of apple juice and domestic washing detergent industries were evaluated.
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Se caracterizaron los extractos etanólicos de hojas y cortezas de 13 especies de la familia Lauraceae mediante cromatografía en capa fina de dos dimensiones (2D-CCD). Los datos posteriores se analizaron mediante técnicas de análisis estadístico multivariado (cluster y análisis de componentes principales (PCA)). Lo anterior permitió hacer una distinción entre los extractos obtenidos de diferentes partes de la planta (hojas y cortezas). Se observó, además, que la metodología usada es capaz de diferenciar entre extractos obtenidos a partir de especies de Lauraceae y los de otras familias de plantas.
Leaves and barks ethanolic extracts from 13 Lauraceae species were characterized through two-dimensional thin layer chromatography (2D-TLC). The subsequent data was analized through multivariate statistical analysis techniques (cluster analysis and principal components analysis (PCA)). This allowed to do a distinction between extracts obtained from different parts of the plant (leaves and bark). In addition, it was observed that the implemented methodology is able to differentiate between extracts obtained from Lauraceae species and some obtained from other plant families.
Caracterizaram-se os extratos etanólicos de folhas e casca obtidos a partir de espécies da família Lauraceae por cromatografia em camada fina em duas dimensões (2D-CCF). Os dados obtidos foram analisados utilizando técnicas de análise estatística multivariada tipo análise de cluster e análise de componentes principais (PCA). As técnicas estadísticas permitiram fazer uma distinção entre os extratos obtidos a partir de diferentes partes da planta (folhas e casca). Além disso, observou-se que o método utilização é capaz de diferenciar entre os extratos provenientes de espécies de Lauraceae daqueles obtidos a partir de outras famílias de plantas.
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Objective To establish a thin-layer chrometograrrgy(TLC) method for the identification of quercetin and chlorogenic acid in Ramulus mori, and to screen their antioxidant activity. Methods The quercetin and chlorogenic acid were extracted by ultrasonic method with methanol as a solvent. The effect of different developed system, reagent, temperature, view methods and different silica gel plate on the TLC of quercetin and chlorogenic acid in Ramulus mori were tested to select the best TLC conditions. The antioxidant activity of quercetin and chlorogenic acid was screened with DPPH as a reagent. Results The ethyl acetate:water:formic acid:toluene(17:2:2:0.8) was used as a developing system and 1% AlCl3 as a chromogenic reagent. Quercetin and chlorogenic acid in Ramulus mori were identified under 366 nm, with blue and blue-green spots on silica gel G plate, and yellowish spots under purple background by the test of TLC-bioautography. Both were proven to have antioxidant activity. Conclusion The method is simple, accurate and reliable, and can be used for quality control of Ramulus mori.
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Objective To establish a thin-layer chrometograrrgy(TLC)method for the identification of quercetin and chloro?genic acid in Ramulus mori,and to screen their antioxidant activity. Methods The quercetin and chlorogenic acid were extracted by ultrasonic method with methanol as a solvent. The effect of different developed system,reagent,temperature,view methods and differ?ent silica gel plate on the TLC of quercetin and chlorogenic acid in Ramulus mori were tested to select the best TLC conditions. The antioxidant activity of quercetin and chlorogenic acid was screened with DPPH as a reagent. Results The ethyl acetate∶water∶formic acid∶toluene(17∶2∶2∶0.8)was used as a developing system and 1%AlCl3 as a chromogenic reagent. Quercetin and chlorogenic acid in Ramulus mori were identified under 366 nm,with blue and blue-green spots on silica gel G plate,and yellowish spots under purple background by the test of TLC-bioautography. Both were proven to have antioxidant activity. Conclusion The method is simple,accu?rate and reliable,and can be used for quality control of Ramulus mori.
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The growing trade market in herbal medicines is aworldwide phenomenon due to several factors, fromthe high cost of manufactured drugs to mere fashion.In this study, we tested the quality of pharmaceuticalproducts based on Hypericum perforatum L. (Eng. ?StJohn?s Wort?) marketed in Divinópolis City, State ofMinas Gerais, Brazil. Samples of products labeled H.perforatum were purchased at three commercial stores,at various times during one year. We assessed thefollowing items: pharmacobotanical characteristics,humidity, total ash, hypericin content and thin layerchromatographic profile. Close inspection showed that4 of the 12 samples sold as H. perforatum products werefrom a different plant from that advertised, representinga forgery in which the true species was replaced byAgeratum sp. Besides, the samples did not entirely meetthe legal requirements for herbal medicine. Therefore,there is a need to strengthen pharmaceutical vigilance,to ensure that herbal products are suitable for publicuse.
O crescente comércio de plantas medicinais e fitoterápicos ocorre em todo o mundo em razão de diversos fatores, como o alto custo dos medicamentos industrializados ou modismo. Neste trabalho verificou-se a qualidade de produtos farmacêuticos contendo Hypericum perforatum L. comercializados em Divinópolis, Minas Gerais, Brasil. Adquiriram-se amostras de H. perforatum em três estabelecimentos distintos em diferentes épocas ao longo de um ano. Avaliaram-se os seguintes itens: aspectos farmacobotânicos, umidade, cinzas totais, doseamento de hipericina e cromatografia em camada delgada. Os resultados demonstraram que quatro amostras comercializadas como H. perforatum eram produtos diferentes daqueles anunciados, caracterizando uma falsificação e substituição da espécie verdadeira por Ageratum sp. Além disso, as amostras não cumpriram totalmente os requisitos exigidos pela legislação. Portanto, faz-se necessário reforçar a vigilância farmacêutica, buscando garantir produtos de qualidade adequados ao uso da população.
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Plantas medicinais são utilizadas mundialmente como uma das principais formas de cuidado primário de saúde. No entanto, a literatura indica que muitas espécies podem apresentar composição química variável, toxicidade ou difícil identificação. O objetivo do presente estudo foi obter critérios úteis para o controle de qualidade farmacognóstico das principais espécies vegetais de uso popular no estado do Rio Grande do Norte, utilizando metodologias de análise botânica (morfodiagnose macro e microscópica) e química (triagem fitoquímica e cromatografia em camada delgada), evitando assim adulterações ou uso inadequado dessas plantas medicinais no estado. No total, sete espécies foram analisadas Acmella oleracea, Chenopodium ambrosioides, Lippia alba, Mentha piperita, Ocimum gratissimum, Peumus boldus e Rosmarinus officinalis. Diversos marcadores botânicos e fitoquímicos foram identificados, contribuindo dessa forma para a correta identificação destas espécies de plantas medicinais importantes no estado do Rio Grande do Norte.
Medicinal plants are worldwide used as one of the main forms of primary healthcare. However, the literature indicates that many species may have variable chemical composition, toxicity, or even difficult identification. The aim of this study was to obtain useful criteria for pharmacognostic quality control of the main plant species of popular use in the state of Rio Grande do Norte, using methods of botanical (macro and microscopic morphodiagnosis) and chemical (phytochemical screening and thin-layer chromatography) analysis, thus preventing adulteration or inappropriate use of these medicinal plants in the state. In total, seven species were analyzed Acmella oleracea, Chenopodium ambrosioides, Lippia alba, Mentha piperita, Ocimum gratissimum, Peumus boldus and Rosmarinus officinalis. Several botanical and phytochemical markers were identified, thereby contributing to the correct identification of these important medicinal plant species in the state of Rio Grande do Norte.
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Plants, Medicinal/metabolism , Quality Control , Botany/methods , /methods , Chromatography, Thin Layer/methodsABSTRACT
Butachlor, a selective systemic herbicide, was isolated, analyzed and detected in viscera obtained from medi-colegal autopsy. Butachlor was extracted by using solvent extraction methods and then identified by Thin Layer Chromatography (TLC). For chromatographic separation, various solvent systems were used. Bromophenol blue was used as chromogenic reagent on developed TLC plates which successfully increased the sensitivity without dispensing with the simplicity of the method. For the study, a total of 15 solvent systems in different ratios were chosen. Of these, the best two solvent systems, namely, Benzene:Diethyl ether (8.5:1.5) and Hexane: Acetone (9:1) were chosen for statistical analysis, which included the calculation of mean Rf value and value of standard deviation and coefficient of variance.
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Objective To develop a method for the determination of Hesperidin,magnolol from "He-Wei-Yin" Mixture,and for its quality control,high-performance liquid chromatography (HPLC) is used.Method After plenty of study about the condition,the final result choosed was as following:an analytical column of HypersiC18(200mm?4.6mm,5?m ) maked by HP was utilized. The column number was 13164421196.The mobile phase was adapted gradient with methanol-1% acetum solution,according to the following profile:0～30min,methanol concentration from 30% to 70%;30～40min,from 70% to 80%;40～50min,from 80% to 30%. The flow rate was 1.0ml/min with the column kept at ambient temperature. All the components had come out in 45 min with the detection wavelength at 294nm. It followed the order of Heperidin,Magnolol according to the retention times in the chromatography.Results In the result,the regression equations were as following:Hesperidin was Y=139.718X+4.511 with a good linearity (r=0.99994). Magnolol was Y=1456.342X+106.506 with a good linearity (r=0.99957) between the peak area and the mass of the standard.The recoveries of the method were as following:in the "He-Wei-Yin" Mixture,for hesperidin,precision of the method RSD=1.87%(n=5),recovery of the method 96.53%(RSD=3.36%,n=3);for Magnolol,precision of the method RSD = 0.34% (n=5); recovery of themethod 93.17%(RSD=4.69%,n=3).At the same condition as above,the determination of content was carried out for six different dose and batch No.Conclusion The method is simple and reliable,easy to operate,suitable for the quality control of Hesperidin and Magnolol in "He-Wei-Yin" Mixture.
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Catechol-type siderophores secreted by a strain of soil bacteria in three different medium were assayed by two high-resolution TLC.The results showed different medium had a significant effect on the secretion of catechol-type siderophores,and in three different medium strain S1 produced different catechol-type siderophores.The effect of Al~(3+) on Catechol-type siderophores by S1 were also assayed.The results showed Al~(3+)had a significant stimulation on the secretion of catechol-type siderophores.Moreover,Al~(3+)could to some extent counteract the repression of Fe~(2+)on siderophores production.In KMB medium four catechol-type siderophores were identified and all ones except for 2,3-dihydroxybenzoic acid(2,3-DHBA) had high affinity for Al~(3+).
ABSTRACT
OBJECTIVE:To study the in vitro and in vivo metabolism of DX by intestinal bacteria in rats and volunteers and the active components in serum of rat after oral administration of DX 900mg/kg METHODS:To detect DX and its metabolites in stool,urine and serum with TLC and EST-MS RESULTS:In vitro,DX was decomposed easily by rat and human intestinal bacteria,and various metabolites were found With prolongation of metablism,metabolite with molecular weight of 415 3 was shown to be corresponding to diosgenin in rat serum and in urine of rats and volunteers CONCLUSION:The above-mentioned DX was decomposed easily by intestinal bacterias and diosgenin was absorbed into serum after oral administration of DX