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One undescribed diterpenoid acid and six compounds were isolated from the 95% ethanol fraction of Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui resin by using various chromatographic methods, including MCI Gel, Sephadex LH-20, ODS, silica gel and semi-preparative HPLC. The planar structures were identified by spectroscopy methods (1D, 2D NMR, UV, IR, MS, etc.), and the absolute configuration of the new compound was determined by ECD calculation. Compound 1 is a new compound, and compounds 2, 5-7 were isolated from Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui for the first time.
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Objective: To establish an HPLC method for the simultaneous determination of syringin, chlorogenic acid, caffeic acid, p-coumaric acid, ferulic acid, ethylsyringin, ethylconiferin, (+)-fraxinol, (±)-rosin, (±)-syringin, taiwanin C, savinin, helioxanthin, and (-)-sesamin in 16 species and 33 batches of Acanthopanax plants. Methods: Separation was carried out on Promosil C18 column (250 mm × 4.6 mm, 5 μm), the mobile phase was eluted with acetonitrile-0.1% phosphoric acid. The flow rate was 1 mL/min, and the column temperature was 30 ℃, the detection wavelength was 280 nm. Results: Under the optimized chromatographic conditions, the linear relationship of the 14 constituents was good in the range of mass concentration, r was more than 0.999 1, with good precision, stability, repeatability and recovery. Conclusion: HPLC method established in this study is effective, accurate, and reproducible and can be used for the simultaneous determination of phenylpropanoids in Acanthopanax plants, which can provide reference for the further study of Acanthopanax plants.
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ABSTRACT Amaranth flour is of high nutritional value, which makes it a potential food. Grinding of the grains is a necessary operation to obtain products with physical properties that provide the food products with adequate characteristics. To analyze the effect of grinding velocity and time on the particle diameters and physical properties of Amaranth flour by ball mill, a Doehlert design with triplicate at the central point was used. The tests were carried out with the mass ratio (balls/samples) (R1:5). Granulometry curve of each design system was fitted to the Rosin-Ramler-Bennet and Holmes-Hukki equations. A found a very significant effect of the velocity on the particle diameters (D50, D63 and D80). The flour obtained were modeled satisfactorily (r2>0.99) by using the Rosin-Ramler-Bennet equation, where the homogeneity index of (n1) was obtained, which was directly influenced by the milling energy. By using the Holmes-Hukki model, were able to model the characteristic diameters with the grinding energy; a critical region was observed between 100μm and 200μm, where lost efficiency in the size reduction. The excess energy, released in the critical region, caused the decrease in starch crystallinity and structural changes in the protein, which affect the functional properties of the flour. The planetary mill is emerging as an effective mean of modifying the functional properties in the development of new food products.
RESUMEN La harina de amaranto es de alto valor nutricional, convirtiéndola en un alimento potencial. La molienda de los granos es una operación necesaria, para brindarle a los productos alimenticios unas adecuadas propiedades físicas. Para analizar el efecto de la velocidad y el tiempo de molienda sobre el diámetro de particular y las propiedades físicas de la harina obtenida por molienda de bolas, se usó un diseño experimental Doehlert, con réplica en el punto central. En las pruebas de molinería se tuvo en cuenta la relación masa de bolas/masa de muestra (R1:5). Las curvas de granulometría de cada punto del diseño experimental fueron modeladas por las ecuaciones de Rosin-Ramler-Bennet y Holmes-Hukki. Se encontró un efecto muy significativo de la velocidad de molienda sobre los diámetros característicos (D50, D63 y D80). El modelo de Rosin-Ramler-Bennet ajustó satisfactoriamente (r2>0.99), además, se obtuvo el índice de homogeneidad (n1), el cual, fue afectado directamente por la energía de molienda. El uso del modelo de Holmes-Hukki permitió relacionar el diámetro de partícula con la energía de molienda y se logró observar una región crítica entre 100μm y 200μm, donde hay una reducción en la eficiencia de la reducción de tamaño de partícula. El exceso de energía liberada en la región crítica causó el descenso en la cristalinidad del almidón y provocó cambios en la estructura de las proteínas, lo cual, modificó las propiedades físicas de la harina. El Molino planetario es una técnica emergente y efectiva para modificar las propiedades funcionales en el desarrollo de nuevo productos alimenticios.
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Objective To investigate the chemical constituents from the seeds of Cuminum cyminum. Methods The chemical constituents were isolated and purified by repeated silica gel column chromatography, Sephadex LH-20 gel column chromatography, medium pressure column chromatography, high pressure flash chromatography, and semi-preparative HPLC, and their structures were elucidated on the basis of physico-chemical constants and spectral analysis. Results Fifteen compounds were identified as astragaline (1), 6-β-hydroxy glycyrrhetinic acid (2), ursolic acid (3), quercetin (4), protocatechuic acid (5), (6R,7E,9R)-9-hydroxy-4,7- megastigma-dien-3-one (6), 4,5-dicaffeoylquinic acid methyl ester (7), 3,5-dicaffeoylquinic acid methyl ester (8), rosin (9), kaempferol 3-O-β-D-glucopyranosyl (1→2)-β-D-glucopyranoside-7-O-α-L-rhamnopyranoside (10), cuminacid (11), cuminoside A (12), luteolin (13), apigenin-7-O-β-D-(6″-O-acetyl)-glucopyranoside (14), and 5,7,4’-trihydroxyflavanone (15). Conclusion Compounds 2, 3, 6-10, and 14 are obtained from this genus for the first time.
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OBJECTIVE: To establish a method for simultaneous determination of five components in wild and tissue-culture materials of Rhodiola crenulata. METHODS: The determination was performed on a Thermo-C18 column (4.6 mm×250 mm, 5 μm) with mobile phase composed of methanol-water (32:68) at a flow rate of 0.8 mL·min-1. The injection volume was 10 μL, column temperature was set at 30℃, and the detection wavelength was set at 277 nm at 0-13 min and 250 nm at 13-60 min. RESULTS: There were linear relationships between the peak areas and contents of salidroside, p-tyrosol, rosarin, rosavin and rosin in the ranges of 2.80-280.00 (r=0.9998), 2.80-280.00 (r=0.9997), 1.20-120.00 (r=0.9996), 1.60-160.00 (r=0.9997) and 1.20-120.00 μg·mL-1 (r=0.9997), respectively. The extraction recoveries varied from 99. 32% to 100.45%. CONCLUSION: The established method is simple and accurate for quality control of wild and tissue-culture materials of Rhodiola.
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OBJECTIVE:To establish a method for the content determination of rosin acid in Rheumatoid arthritis tablet. METH-ODS:HPLC was performed on the column of ZORBAX SB-C18 with mobile phase of acetonitrile-0.1% formic acid(82∶18,V/V) at flow rate of 1.0 ml/min ,detection wavelength was 241 nm ,column temperature was 30 ℃ and volume injection was 10 μl. MS/MS column was ZORBAX SB-C18 with mobile phase of acetonitrile-0.1% formic acid(80∶20,V/V)at flow rate of 0.2 ml/min;column temperature was 30 ℃;volume injection was 0.5 μl. Ionization mode was ESI+,atomization gas pressure was 25 psi,gas flow as 8.0 L/min,capillary voltage was 4 000 V,capillary outlet voltage was 120 V,precursor ion was 303 m/z,scan range was 50-500 m/z and the gas temperature was 350 ℃. RESULTS:The linear range of rosin acid was 2.5-100.0 μg/ml. RSDs of preci-sion,stability and reproducibility tests were lower than 2.0%,recoveries was 96.75%-98.11%(RSD=0.53%,n=6). CONCLU-SIONS:The method is simple,accurate and reproducible,and suitable for the content determination of rosin acid in Rheumatoid arthritis tablet.
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ObjectTo develop the reliable RP-HPLC methods for the determination of salidroside, tyrosol, rosavin, rosin, and rosarin in the plants of Rhodiola L. and to evaluate their species from different habitats. Methods Method Ⅰ: methanol-water (0.5 mmol/L SDS in 1% acetic acid aqueous solution) system for the analysis of salidroside; method Ⅱ: acetonitrile-water system for rosavin; method Ⅲ: aqueous acetonitrile-phosphoric gradient system for salidroside, tyrosol, rosavin, rosin, and rosarin. Results The contents of salidroside in different species range from 0.021% to 1.420%, and those of rosavin in all species are very limited or undetected except in Rhodiola rosea L. and R. sachalinensis. The contents of the five marker ingredients are significantly species- and habitat-dependent. Conclusion Three RP-HPLC methods are established for quantitative analysis of the above five marker ingredients in the meantime, respectively. Evaluation of the quality of varied species of Rhodiola L. shows that R. rosea growing in Xinjiang Uygur Autonomous Region and R. sachalinensis growing in Jilin province are the two better species contained with abundant above-mentioned ingredients in China.