ABSTRACT
SUMMARY Franz cells are one of the main tools to evaluate the transepithelial permeation of compounds through the performance of in vitro tests, these allows inferring the safety behavior of a compound in the skin. The objective of this research was to determine the permeation behavior of benzoic acid from complexes with polyelectrolytes (EuB 75 Cl 25 EuB 100), compared to benzoic acid without complexing, to infer its safety behavior. In a first phase, skin storage conditions were established comparatively evaluating the diffusion parameters (flow and permeation constant) and transepithelial water loss, using ears skin of freshly slaughtered pigs, stored in 1M NaCl at -2 °C for 3 days; it was worked under infinite doses conditions. Subsequently, the permeation test of two complexes between Eudragit E and benzoic acid, in comparison with benzoic acid, was carried out under finite dose conditions. The benzoic acid quantification was performed with an analytical method validated by HPLC-DAD. The results showed no significant differences showing that biological samples can be stored for 72 h under the conditions described. The permeation behavior of the complexed benzoic acid with respect to the free benzoic acid showed a better safety profile, since there was a lower permeation for the first case. These results show that complexation of benzoic acid could decrease the sensitivity reactions that it normally presents, based on the decrease in its permeation.
RESUMEN Las celdas de Franz son una de las herramientas para evaluar la permeación transe-pitelial de compuestos mediante la realización de ensayos in vitro, estos permiten inferir el comportamiento de seguridad de un compuesto en la piel. El objetivo de esta investigación fue determinar el comportamiento de permeación del ácido benzoico a partir de complejos con polielectrolitos (EuB 75 Cl 25 EuB 100) en comparación con el ácido benzoico sin complejar, para inferir su comportamiento de seguridad. En una primera fase, se establecieron las condiciones de almacenamiento de la piel comparando los parámetros de difusión (flujo y constante de permeación) y pérdida de agua transepitelial, empleando piel de orejas de cerdos recién sacrificados, almacenadas en NaCl 1M a -2°C por 3 días; se trabajó bajo condiciones de dosis infinitas. Posteriormente, se realizó el ensayo de permeación de dos complejos entre ácido benzoico y Eudragit E, en comparación con el ácido benzoico, bajo condiciones de dosis finitas. La cuantificación del ácido benzoico fue realizada con un método analítico validado por HPLC-DAD. Los resultados evidenciaron que las muestras biológicas pueden almacenarse durante 72 h en las condiciones descritas. El comportamiento de permeación del ácido benzoico complejado respecto al ácido benzoico libre demostró tener un mejor perfil de seguridad, puesto que hubo una menor permeación para el primer caso. Estos resultados demuestran que la complejación del ácido benzoico podría disminuir las reacciones de sensibilidad que normalmente este presenta, basándose en la disminución de su permeación.
ABSTRACT
RESUMEN Se desarrolló y validó un método por cromatografía gaseosa para la cuantificación simultánea de mentol (MT), salicilato de metilo (SM), timol (TM) y ácido benzoico (AB) en una solución antiséptica bucal. Se utilizó una columna DB-WAX y dietilenglicol como estándar interno. Se determinó la linealidad en un intervalo de concentraciones de 64,00 a 96,00 µg/mL (MT), 80,00 a 120,00 µg/mL (SM), 96,00 a 144,00 µg/mL (TM) y 48,00 a 72,00 µg/mL (AB), obteniendo coeficientes de correlación superiores a 0,999, y coeficientes de variación de los factores de respuestas de 1,18, 1,95, 3,52 y 1,48%, respectivamente. Se establecieron límites de detección de 0,51; 1,14; 3,34 y 1,402 ng/mL para el MT, SM, TM y AB, respectivamente, mientras los límites de cuantificación fueron de 1,45, 3, 43, 9, 73 y 4, 36 ng/mL en cada caso. Los porcentajes de recuperación fueron de 100,03, 99, 31, 99, 92 y 100,12; con coeficientes de variación de 0,42, 0,79, 0,66 y 0,76% para cada caso. El método fue lineal, exacto, preciso y selectivo para la determinación de los analitos en el control de calidad.
SUMMARY A method was developed and validated by gas chromatography for the simultaneous quantification of menthol (MT), methyl salicylate (SM), thymol (TM) and benzoic acid (AB) in an oral antiseptic solution. A DB-WAX column and diethylene glycol was used as internal standard. Linearity was determined in a concentration range of 64.00 to 96.00 µg/mL (MT), 80.00 to 120.00 µg/mL (SM), 96.00 to 144.00 µg/mL (TM) and 48.00 to 72.00 µg/mL (AB) achieving correlation coefficients greater than 0.999, and coefficients of variation of the response factors of 1.18, 1.95, 3.52 and 1.48%, respectively. Detection limits were established: 0.51, 1.14, 3.34 and 1.402 ng/mL for MT, SM, TM, and AB, respectively, while the quantification limits were 1.45, 3.43, 9.73 and 4.36 ng/mL in each case. Recovery percentages were 100.03, 99.31, 99.92 and 100.12; with coefficients of variation of 0.42, 0.79, 0.66 and 0.76% for each case. The method was linear, accurate, precise, and selective for the determination of analytes in quality control.
ABSTRACT
Objective: To study the chemical constituents of the Eupatorium adenophorum. Methods: The chemical constituents were isolated and purified by silica gel chromatography repeatedly from the ethyl acetate extract of E. adenophorum, and their structures were identified by spectral analysis and chemical methods. Results: Fourteen compounds were isolated from E. adenophorum and identified as p-hydroxybenzoic acid ethyl ester (1), (1R,4R)-8aα-hydroxy-1-isopropyl-4,7-dimethyl- 1,2,3,4,6,8a-hexahydro-naphthalene-2,6-dione (2), daedalin A (3), 10-oxo-7-hydroxy-nordehydrotremetone (4), caffeoyl acetate (5), syringic acid (6), 3-hydroxy-4-(1-oxo-ethane)-benzoic acid (7), ferulic acid (8), p-hydroxyphenylethyl alcohol (9), protocatechuic acid ethyl ester (10), 4-hydroxy-3-isopropyl benzoic acid (11), balanophonin (12), indole-3-carboxylic acid (13), and 6-methoxy kaempferol (14). Conclusion: Compound 11 is obtained from natural products for the first time, compounds 1, 3, 6, 7, 9, 10, 12-14 are obtained from this genus for the first time, and compound 5 is obtained from this plant for the first time.
ABSTRACT
@#Introduction: The quality of Zinc Oxide Eugenol-Ethoxy Benzoic Acid (ZOE-EBA) dental cement could be improved by the addition of Aluminum Oxide (Al2 O3 ). It was caused by the characteristic of alumina which are easy on fabrication process, resistant on corrosion, endurance usage, bioinert, and biocompatible. The purpose of this study was to determine the effect of the addition of Al2 O3 in ZOE-EBA cement. Methods: Nanoparticle of ZnO (zinc oxide), Al2 O3 , MgO (magnesium oxide),eugenol liquid and EBA (Ethoxy Benzoic Acid) fluid. The variations of Al2 O3 were 24%, 26%, 28%, 30%. First is the sintering on 1000°C and tested by XRD. Sintered powder was mixed with liquid, with a ratio of powder: liquid 7:1. The mechanical characteristic are compressive strength and hardness. Results: XRD test is showed that ZnO has dominant phase on the sample and there was new phase on cement powder such as Zinc-Aluminium oxide (ZnAl2 O4 ). The best result was shown on the addition of 26% of Al2 O3 composition in the 3 type test because the sample had ZnAl2 O4 phase volume fewer than 28% and 30% of Al2 O3 . This result was supported by the compressive strength and hardness which showed the optimum value at concentrations of 26%, which were 64.49 MPa and hardness of 69.33 VHN. Conclusion: Based on the result, it was found that Al2 O3 variation gives the best results in the teeth ZOE-EBA cement was 26%.
ABSTRACT
Aim To study the material basis of hepatotoxicity induced by the ripe fruit of Terminalia chebula Retz. var. tomentella Kurt using high content screening. Methods Shikimic acid, benzoic acid, gallic acid, and 1,2,3,4,6-o-pentagalactosyl glucose were applied to HepG2 cells, respectively, and the cells were stained with fluorescent stains such as Hoechst 33342. The imagewas scannedand the collected datawere input into the Assay Template. Finally, the dose-response curves of cell numbers, DNA content, GSH reduction level, ROS content, MMP and other indicators were obtained for different monomers at different concentrations, thereby the hepatotoxicity of the monomers was determined. Results Aspirin and shikimic acid showed negative results. Ticlopidine, benzoic acid, 1,2,3,4,6-o-pentagalloglucose, gallic acid caused a significant decrease in cell number and increase in ROS content. There was a risk of liver-toxicity. Conclusions Gallic acid, benzoic acid, 1,2,3,4,6-o-pentagalactosylglucose have the risk of hepatotoxicity, and the risk of hepatotoxicity caused by gallic acid is the largest. Basically, gallic acid is safer when administered at concentrations below 50 mg·L-1
ABSTRACT
RESUMEN La obtención de complejos polielectrolito entre el polímero catiónico Eudragit® E100 y moléculas aniónicas, con neutralización adicional de un ácido inorgánico, ha sido una práctica recurrente en el área de investigación de estos sistemas de liberación controlada. En el presente trabajo se buscó estudiar el efecto de la adición del ácido fuerte en el polímero, para ello se llevó a cabo la obtención por evaporación de solvente de diez complejos (de diferente composición entre Eudragit® E100 y ácido benzoico o ácido clorhídrico) y de cuatro ionómeros (sin el activo), a los cuales se les realizó análisis por FTIR y DSC. Los resultados demostraron la obtención de los respectivos complejos polielectro-lito y de los ionómeros; además los espectros de FTIR revelaron la relación directa entre la reacción de hidrólisis de los grupos ésteres del polímero y la proporción de HCl adicionada. Los termogramas, por su parte, evidenciaron la existencia de una reacción en el polielectrolito (PE), la cual se favoreció en aquellas composiciones en las que el proceso de hidrólisis ocurrió en mayor magnitud. El proceso de hidrólisis que se describe en el presente estudio debe tenerse en consideración en las futuras investigaciones en el campo, ya que su ocurrencia podría tener implicaciones en las diversas variables que se evalúan en este tipo de sistemas.
SUMMARY Polyelectrolyte complexes obtention between Eudragit® E100 (cationic polymer) and anionic molecules with additional neutralization of inorganic acids is a common practice in the development of these systems. In the present work the addition of strong acid effect on polymer structure was evaluated through FTIR and DSC analysis of a set of ten complexes with different composition (between Eudragit® E100 and benzoic acid) and four ionomers (without the preservative) obtained by solvent evaporation technique. Results demonstrated the complexes and ionomers formation. FTIR spectra revealed direct relationship between polymer ester groups hydrolysis reaction and the amount of HCl added. The thermograms, on the other hand, evidenced the existence of a reaction in the polyelectrolyte, which was favored in those compositions with more hydrolysis process. The degradation reaction described in this study should be taken into consideration in future research, since its occurrence could have implications in variables evaluated in this type of systems.
ABSTRACT
Objective To evaluate the effects of 15 kinds of drying methods including sun-drying, shade drying, infrared drying (50, 60, 70, 80 ℃), microwave drying (50, 60, 70, 80, 100 ℃), and hot-air drying (50, 60, 70, 80 ℃) on the quality of Leonurus japonicus through the content of multiple chemical components, and then optimize suitable drying methods for L. japonicus. Methods UPLC-QTRAP®/MS2 method was developed to determine the content of three alkaloids (stachydrine hydrochloride, leonurine hydrochloride, trigonelline), four phenolic acids (benzoic acid, p-hydroxybenzoic acid, vanillic acid, syringic acid), five phenylpropanoids (salidroside, acteoside, chlorogenic acid, caffeic acid, ferulic acid), 11 flavonoids (rutin, isoquercitrin, hyperoside, wogonin, kaempferol-3-O-rutinoside, genkwanin, apigenin, kaempferol, isorhamnetin, hesperetin, quercetin), and one iridoid glycoside (ajugol) in L. japonicus. The principal component analysis (PCA) and TOPSIS analysis were performed to evaluate the quality of the L. japonicus samples obtained by different drying methods. Results Different drying methods exerted significant effects on the content of 24 chemical ingredients in L. japonicus. The PCA analysis divided 15 drying methods into three types based on the content of 24 compounds. Moreover, the comprehensive evaluation of TOPSIS was carried out, and the top three drying methods were 70 ℃ hot-air drying, 60 ℃ hot-air drying, and 100 ℃ microwave drying, which largely retained the active ingredients of L. japonicus. Conclusion Combined with practice, we found that 70 ℃ hot-air drying was the optimized drying process of L. japonicus, which provides guarantee for the quality of L. japonicus and provides scientific basis for the production and processing of L. japonicus.
ABSTRACT
Objective To study the chemical constituents from the rhizomes of Securidaca inappendiculata. Methods The concrete exacted by 95% EtOH from the rhizomes of S. inappendiculata was isolated and purified by chromatography on macroporous resin, silica gel, MPLC, gel, preparative HPLC, etc. The structures of the chemical constituents were elucidated by means of physicochemical properties and spectroscopic analysis. Results Five compounds were isolated and identified as 2- methylene-butanoic acid 4-O-[(β-D-glucopyranosyl)oxy]-intramol-1,6’-ester (1), 3-methoxyl-4-O-β-D-glucopyranosyloxy-benzoic acid methyl ester (2), threo-4,7,9,9’-tetrahydroxy-3,3’-dimethoxy-8-O-4’-neolignan-4-O-β-D-glucopyranoside (3), eucomegastigside A (4), and acernikol-4″-O-β-D-glucopyranoside (5). Conclusion Compound 1 is a new hemiterpene glycoside named securiterpenoside D, and compounds 2-4 are isolated from Polygalaceae for the first time.
ABSTRACT
To isolate and identify the chemical constituents from the rhizome of Cimicifuga dahurica. Methods The isolation and purification of 60% EtOH extract of the rhizomes of C. dahurica were carried out through various modern chromatographic separation techniques: HP-20, silica gel, ODS, Sephadex LH-20 column and semi-preparative HPLC. And the structures of the compounds were identified based on spectroscopic data and physicochemical properties. Results Twenty compounds were isolated and identified as cimicifugaside F (1), (+) (2S,3R)-2-(4-hydroxy-3-methoxyphenyl)-3-[(β-D-glucopyranosyloxy) methyl]-7-methoxybenzofuran-5-propenoic acid (2), 5-hydroxy-2-methoxybenzoic acid (3), benzoic acid 4-O-β-D-glucoside (4), isoferulic acid (5), ferulic acid (6), trans-ferulic acid 4-O-β-D-allopyranoside (7), trans-ferulic acid 4-O-β-D-glucoside (8), (E)-sinapic acid 4-O-β-D-glucoside (9), 6,6’-di-O-sinapoylsurcose (10), piscidic acid (11), fukinolic acid (12), N-trans-feruloyltyramine 4-O-β-D-allopyranoside (13), N-trans-3’-methoxy-4’-feruloyltyramine-4-O-β-D-allopyranoside (14), N-trans-3’-methoxy-4’- feruloyltyramine-4-O-β-D-glucoside (15), grevilloside G (16), (-)-syringaresinol (17), (-)-syringaresinol 4,4’-di-O-β-D- allopyranoside (18), (+)-isolarisiresinol 3a-O-β-D-glucoside (19), (-)-5’-methoxyisolariciresinol 3a-O-β-D-glucoside (20). Conclusion Compound 1 was identified as a new lignan, and compounds 2-4, 8-10, 15-17 and 20 were isolated from Cimicifuga genus for the first time.
ABSTRACT
Objective: To establish HPLC coupled with wavelength switching and gradient elution method (HPLC-DVD) for simultaneous determination of 14 active components (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, geniposide, 4-hydroxyacetophenone, scutellarin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, oroxylin A 7-O-glucuronide, wogonoside, baicalein, wogonin and oroxylin A and one auxiliary material (benzoic acid) in Yinzhihuang Oral Solution (YOS). Methods: The chromatographic separation was achieved on Welch Ultimate XB-C18 (250 mm × 4.6 mm, 5 μm) column with acetonitrile-0.1% phosphoric acid solution as mobile phases for gradient elution, at the flow rate of 0.8 mL/min in the first 30 min and 1.0 mL/min in the follow-up; The detection wavelength was set at 325 nm for neochlorogenic acid, chlorogenic acid and cryptochlorogenic acid, 238 nm for geniposide, 275 nm for 4-hydroxyacetophenone, 228 nm for benzoic acid, 325 nm for scutellarin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C, 203 nm for oroxylin A 7-O-glucuronide and wogonoside, and 274 nm for baicalein, wogonin and oroxylin A. The volume of sample injection was 10 μL. Results: The fifteen active components were well separated and showed good linearity, such as neochlorogenic acid 74.46-1 574.42 ng (r = 0.999 8), chlorogenic acid 34.58-741.1 ng (r = 0.999 6), cryptochlorogenic acid 34.65-742.62 ng (r = 0.999 7), geniposide 234.42-5 024.45 ng (r = 0.999 9), 4-hydroxyacetophenone 74.46-1 574.42 ng (r = 0.999 9), benzoic acid 321.79-6 897.1 ng (r = 0.999 8), scutellarin 44.7-958.08 ng (r = 0.999 7), isochlorogenic acid B 32.53-697.22 ng (r = 0.999 5), isochlorogenic acid A 8.6-184.38 ng (r = 0.999 6), isochlorogenic acid C 31.93-684.3 ng (r = 0.999 7), Oroxylin A 7-O-glucuronide 254.82-5 461.66 ng (r = 0.999 5), wogonoside 10.18-218.12 ng (r = 0.999 9), baicalein 92.81-1 989.33 ng (r = 0.999 6), wogonin 31.17-668 ng (r = 0.999 5), and oroxylin A 11.74-251.73 ng (r = 0.999 8). The precision was good, and RSD was not more than 0.75%. The repeatability was good, and the RSD was not more than 1.95%. The stability was good in 8 h, and RSD was not more than 1.77%. The average recoveries and corresponding RSD values were 100.69% (0.55%), 101.99% (1.78%), 99.20% (0.72%), 100.13% (0.48%), 100.96% (1.74%), 100.02% (0.46%), 101.14% (0.27%), 99.87% (0.59%), 100.21% (1.56%), 102.18% (0.33%), 99.00% (1.02%), 98.82% (0.65%), 98.31% (0.58%), 96.01% (0.44%), and 100.56 (0.71%), respectively. The content of 10 batches of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, geniposide, 4-hydroxyacetophenone, benzoic acid, scutellarin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, oroxylin A 7-O-glucuronide, wogonoside, baicalein, wogonin and oroxylin A were 0.246-0.322, 0.213-0.290, 0.203-0.267, 1.786-2.047, 0.035-0.046, 2.393-2.541, 0.263-0.392, 0.139-0.216, 0.032-0.067, 0.208-0.250, 2.120-2.648, 0.063-0.102, 0.081-1.429, 0.164-0.246, and 0.079-0.110 mg/mL. Conclusion: HPLC coupled with wavelength switching and gradient elution method has been established for simultaneous determination of 15 components in YOS. The method is simple, quick, accurate, and it can be used for content determination and quality control of YOS.
ABSTRACT
Objective: To study the fingerprints of Paeoniae Radix Rubra in different habitats, and determine the content of five chemical components (gallic acid, albiflorin, paeoniflorin, benzoic acid, and benzoyl paeoniflorin) and systematically cluster them. The relationship between origin and content was analyzed by grey correlation degree to provide reference for the quality evaluation of Paeoniae Radix Rubra. Methods: Fingerprints of Paeoniae Radix Rubra from 21 different producing areas were constructed by high performance liquid chromatography. The results were classified by principal component analysis and systematic cluster analysis. The gray correlation degree method was used to process the index components and their relative correlations were calculated. Results: HPLC fingerprints of Paeoniae Radix Rubra from 21 habitats were established, 11 common peaks were confirmed, and five of them (gallic acid, albiflorin, paeoniflorin, benzoic acid, and benzoyl paeoniflorin) were identified. The similarity of Paeonia lactiflora was greater than 0.9, and the similarity of Paeonia veitchii was less than 0.9. It was divided into two categories by principal component analysis combined with cluster analysis. The results of grey correlation analysis showed that the relative correlation (ri) was the largest in Gansu, followed by Ganzi in Sichuan. Conclusion: There is a big difference in the relative yield of Paeoniae Radix Rubra in different habitats. This experiment provides a scientific basis for the quality evaluation of Paeoniae Radix Rubra by fingerprint analysis, principal component analysis combined system cluster analysis and grey correlation analysis method.
ABSTRACT
AIM To establish an HPLC method for the simultaneous content determination of five constituents in Baishao Formula Granules (Paeoniae Radix Alba).METHODS The analysis of aqueous extract of this drug was performed on a 30 ℃ thermostatic Phenomenex C18 column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.05％ phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 230 nm.RESULTS Paeoniflorin,albiflorin,paeoniflorin sulfonate,gallic acid and benzoic acid showed good linear relationships within the ranges of 0.020-0.639 mg/mL (r =0.999 8),0.005-0.172 mg/mL (r =0.999 9),0.020-0.652 mg/mL (r =1.000 0),0.003-0.097 mg/mL (r =0.999 8),0.002-0.058 mg/mL (r =0.999 7),whose average recoveries were 99.1％,98.3％,98.6％,98.1％ and 99.5％ with the RSDs of 1.86％,1.37％,1.69％,1.46％ and 2.26％,respectively.The contents of various constituents in twenty-seven batches of samples demonstrated obvious differences.CONCLUSION We should pay attention to Paeoniae Radix Alba in Baishao Formula Granules due to its unstable quality.
ABSTRACT
A new method for simultaneous determination of six benzoic acid esters and their metabolite p-hydroxybenzoic acid (p-HB) in sediments was developed.The samples were extracted with methanol and water,and then the extraction was purified by Oasis MCX solid phase column.The separation of targets was conducted by passing through a UPLC?HSS T3 column with a methanol-0.1% acid aqueous solution as the mobile phase under gradient elution.The qualitative analysis of the analytes was measured by Ultra performance liquid chromatography-Triple quadrupole tandem mass under multiple reaction monitoring mode (MRM) and the internal standard method was applied for quantitative analysis.The results indicated that seven target substances had a good linear relationship in the range of 0.1-500 μg/L with correlation coefficients above 0.9995 and the detection limits of 0.75-1.23 ng/g.The recoveries ranged from 65.5% to 88.3% and the relative standard deviation was 7.4%-13.6%.This method was suitable for the measurement of benzoic acid esters with the advantages such as simple processing,good selectivity and high sensitivity.
ABSTRACT
Objective To develope a high performance liquid chromatography ( HPLC) method for simultaneous determination of benzoic acid and salicylic acid in compound benzoic acid embrocation. Methods An Alltima C18 column (150 mm×4.6 mm,5 μm) was used for the separation, with methanol-0.1％ phosphoric acid (50:50) as the mobile phase at the flow rate of 1.0 mL?min-1 .The detection wavelength was set at 236 nm.The column temperature was 35 ℃ . Results The good linearity was obtained with the correlation coefficient (r) of 1.0000 for benzoic acid and salicylic acid;the precisions and stability were satisfactory, and the relative standard deviations (RSDs) were less than 0.3％.The average recoveries (n= 9) were 100.15％ and 99.85％ for benzoic acid and salicylic acid, respectively. Conclusion The established method is accurate, simple and rapid, and can be utilized for the simultaneous determination of benzoic acid and salicylic acid in compound benzoic acid embrocation.
ABSTRACT
Objective: To develop a RP-ion pair HPLC with wavelength switching for the simultaneous determination of 4 components (marine, oxymarine, salicylic acid, benzoic acid) in Fufang Kusheng Shuiyangsuan powder.Methods: An Agilent ZORBAX SB-C18 column(150 mm× 4.6 mm, 5 μm) was used;the mobile phase was acetonitrile (A)-0.1% phosphoric acid solution (0.2 g sodium heptanesulfonate was added to 100 ml solution) at a flow rate of 1.0 ml·min-1;the detection wavelength was 220 nm in 0-12 min and 280 nm in 12-25 min;the column temperature was 30℃.Results: The linear range of marine, oxymarine, salicylic acid and benzoic acid was 0.006 030-0.120 6 μg (r=0.999 4), 0.016 56-0.331 2 μg (r=0.999 9), 0.717 1-14.34 μg (r=0.999 9) and 0.512 0-10.24 μg (r=0.999 9), respectively;the average recovery was 98.14%, 97.20%, 97.05% and 98.39% with the RSDs of 1.38%, 0.32%, 0.81% and 1.26%(n=6) , respectively.Conclusion: The method is simple and rapid, and can be applied in the simultaneous determination of 4 components in Fufang Kusheng Shuiyangsuan powder.
ABSTRACT
OBJECTIVE: To investigate the chemical constituents in the roots of Allium tuberosum. METHODS: Colum chromatography with different materials such as silica gel was used to isolate and purify the chemical constituents. Their structures were identified by spectroscopic analysis. RESULTS: Nine compounds were isolated from the roots of Allium tuberosum and their structures were identified as 4,8-dihydroxyacetophenone-8-O-ferulate(1), 4,8-dihydroxyacetophenone(2), 3,4,5-trimethoxybenzoic acid(3), 3,4,5-trimethoxycinnamic acid(4), buddlenol D(5), E-1,6,11-triene-4,5,9-trithiadodeca-9,9-dioxide(6), tianshic acid(7), daucosterol(8), and linoleic acid(9). CONCLUSION: Compound 1 is a new compound and compounds 2-5 are obtained from Allium tuberosumfor the first time.
ABSTRACT
Objective: To study the chemical constituents from the stems and leaves of Cirsium henryi. Methods: The chemical constituents were isolated by various chromatography techniques and their structures were elucidated on the basis of spectroscopic analysis. Results: Sixteen compounds were isolated and identified to be stearic acid (1), 2,3-dihydroxypropyl hexadecanoate (2), palmitic acid (3), taraxasterol (4), pseudo taraxasterol (5), taraxa-sterol acetate (6), β-sitosterol (7), daucosterol (8), protocatechuic acid (9), uracil (10), linarin (11), apigenin (12), quercitrin (13), acacetin (14), acacetin-7-O-β-D-glucoside (15), and 4-hydroxy- 3,5-dimethoxy benzoic acid (16), respectively. Conclusion Compounds 3 and 10-16 are isolated from the plant for the first time, and compounds 10, 13, and 16 are isolated from the plants of Cirsium Mill. Emend. Scop. for the first time.
ABSTRACT
OBJECTIVE:To establish amethod for simultaneous determination ofbenzoic acid,methylis salicylas and thymol in Compound thymol solution.METHODS:HPLC was performed on the column of Thermo Hypersil BDS C18 with the mobile phase ofacetonitrile-water-acetic acid(40∶60∶0.02,V/V/V)at a flow rate of 1 ml/min,the detection wavelength was 275 nm,column tem-perature was 30 ℃,and injection volume was 10 μl. RESULTS:The linear range was 0.045 2-0.9030 mg/ml for benzoic acid, 0.0492-0.9844 mg/ml for methylis salicylas and 0.046 4-0.927 0 mg/ml for thymol;RSDs of precision,stability and reproducibility tests were lower than 2%;recoveries were 98.40%-108.88%(RSD=3.26%,n=9),98.21%-104.07%(RSD=1.87%,n=9) and 96.83-107.09%(RSD=3.33%,n=9),respectively. CONCLUSIONS:The method is simple,accurate and specific,and accurately de-termine the contents of benzoic acid,methylis salicylas and thymol in Compound thymol solution.
ABSTRACT
Objective: To investigate the chemical constituents from the whole plant of Incarvillea delavayi. Methods: The whole plant of I. delavayi was extracted by 90% ethanol. Various chromatography methods were employed to separate the chemical constituents, and the structures were identified by comprehensive spectroscopic analysis. Results: Fourteen compounds, including cyclohexanethanoids, monoterpene alkaloids, and triterpenoids, were obtained from the 90% ethanol extract of I. delavayi. Their structures were identified as 5-hydroxyethyl-6-hydroxyl-3-methyl benzofuran (1), cleroindicin B (2), 3,4,5-trimethoxyl benzoic acid ethyl ester (3), 3,4,5-trimethoxyl benzoic acid methyl ester (4), 6-hydroxyl dihydrobenzofuran (5), 2-(4'-ethoxyphenyl)-ethanol (6), tecomine (7), (+)-epidihydrotecomanine (8), 5-hydroxy skytanthine (9), δ-skytanthine (10), isoincarvilline (11), mairine B (12), coelobillardierine (13), and 3β-acetyl oleanolic acid (14). Conclusion: Compound 1 is identified as new compound and named as delavayol A, while compounds 3-6, 9-11, and 13 are isolated from the titled plant for the first time.
ABSTRACT
Objective: To determine the nine components in Shiwei Penan Granule and establish the fingerprnt analysis for the quality control of Shiwei Penan Granule. Methods: The method was performed on a Thermo C18 column (250 mm × 4.6 mm, 5 μm); The gradient mobile phase consisted of acetonitrile (A)-0.1% phosphoric acid (B) with a flow rate of 1.0 mL/min (0-16 min, 5%-14% A; 16-20 min, 14%-17% A, 20-35 min, 17%-19% A; 35-60 min, 19%-35% A; 60-62 min, 35%-75% A; 62-78 min, 75% A); The detection wavelength was set at 230 nm (for quantitative analysis and fingerprint). Results: Gallic acid, sodium danshensu, chlorogenic acid, paeoniflorin, polydatin, benzoic acid, salvianolic acid B, emodin, and physcion were baseline seperated with good linearity relationships (r > 0.999 9) between concentration and peak areas over the linear ranges. The average recoveries of the compounds were 100.15% (RSD = 1.39%), 99.89% (RSD = 1.71%), 99.92% (RSD = 0.67%), 99.28% (RSD = 0.60%), 99.89% (RSD = 0.80%), 99.72% (RSD = 1.83%), 99.91% (RSD = 0.79%), 100.06% (RSD = 0.94%), and 99.97% (RSD = 1.36%). Using Traditional Chinese Medicine Fingerprint Similarity Evaluation System (2012 Edition) to analyze the fingerprint of 15 batches of Shiwei Penan Granule, the similarity values between the reference fingerprint and the 15 batches were higher than 0.977. Conclusion: The method is simple, rapid, and accurate, and can be used as an effective method to evaluate the quality of Shiwei Penan Granule.