ABSTRACT
Objective: To establish HPLC method for the determination of 6'-O-caffeoylarbutin (1), arbutin (2), robustaside A (3), p-hydroxybenzoic acid (4), caffeic acid (5) and caffeic acid methyl ester (6) of Queshe tea. Methods: Using the SunFire® C18 (250 mm×4.6 mm, 5 μm) chromatographic column, mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution, the flow rate at 1.0 mL/min, and column temperature at 30 ℃ to optimum the extraction method of Queshe tea and investigate the linearity, stability and repeatability of the method. Results: With distilled water as the extraction solvent, the highest extraction rate can be obtained by ultrasonic extraction for 20 min. Under the above chromatographic conditions, 6'-O-caffeoylarbutin (1), arbutin (2), robustaside A (3), p-hydroxybenzoic acid (4), caffeic acid (5) and caffeic acid methyl ester (6) have good separation effect, and the experiment has good linearity, stability and repeatability. Conclusion: The method is simple, sensitive and accurate, and can be used for the detection of the above six main chemical components.
ABSTRACT
An RP-HPLC method was established to separate the related substances of benzyl hydroxybenzoate.The separation was carried out on a Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column.The mobile phase was methonal-0.1％ glacial acetic acid,using linear gradient elution,and the detection wavelength was 254 nm.There was a good linear relationship between 0.051-101.88 μg/mL (r =1.00) and 0.050-99.48 μg/mL(r =0.999 8) for benzyl hydroxybenzoate and p-hydroxybenzoic acid,repectively.The average recovery of p-hydroxybenzoic acid was 100.3％ and the RSD was 0.95％.The LOQ of p-hydroxybenzoic acid was 0.24 ng.The detected impurities were also identified by UPLC-Q-TOF.The established method is accurate and reproducible,and could be used for the quality control of benzyl hydroxybenzoate.
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OBJECTIVE: To study the chemical constituents from the leaves of Jiangxi genuine medicinal material Chimonanthus nitens Oliv. METHODS: The compounds were isolated and purified by silica gel column chromatography, Sephadex LH-20, ODS column chromatography, semi-preparative HPLC, and so on. Their structures were elucidated on the basis of physiochemical properties and spectral data. RESULTS: Ten compounds were isolated and elucidated as uracil (1), 6, 7-dimethoxycoumarin (2), 6, 7, 8-trimethoxycoumarin (3), p-hydroxybenzoic acid ethyl ester (4), 1∶1 mixture of two diastereomers identical with (3RS, 6RS)-2, 6-dimethyl-octa-1, 7-dien-3, 6-diol (5 and 6), kaempferol (7), isofraxidin (8), scopoletin (9), and loliolide (10). CONCLUSION: Compounds 1, 3-6 and 10 are isolated from this plant for the first time and compounds 1, 4-6 are isolated from this genus for the first time.
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Objective: To study the chemical constituents of Periploca Radix. Methods: The chemical constituents of Periploca forrestii were separated using various chromatographic techniques. Their structures were elucidated by spectral analysis. Results: Nineteen compounds were isolated from the 70% ethanol extract of P. forrestii, and identified as 3-O-caffeoylquinic acid methyl ester (1), 4-O-caffeoylquinic acid methyl ester (2), 5-O-caffeoylquinic acid methyl ester (3), 3-O-caffeoylquinic acid (4), 4-O-caffeoylquinic acid (5), 5-O-caffeoylquinic acid (6), 1, 3-di-O-caffeoylquinic acid (7), 3, 4-di-O-caffeoylquinic acid (8), 3, 5-di-O- caffeoylquinic acid (9), 4, 5-di-O-caffeoylquinic acid (10), protocatechuic aldehyde (11), p-hydroxybenzoic acid (12), o-hydroxybenzoic acid (13), syringic acid (14), vanillic acid (15), periforgenin A (16), Δ5-pregnene-3β, 17α, 20α-triol (17), periforgenin C (18), and periplogenin (19). Conclusion: Compounds 1-12 are isolated from the plants of genus Periploca Linn. for the first time, and compound 13 is isolated from P. forrestii for the first time.
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Objective: To study the chemical constituents from the aerial parts of Fagopyrum dibotrys. Methods: The compounds were isolated and purified by means of chromatographic techniques and their structures were identified on the basis of spectral features. Results: Fourteen known compounds were isolated in the methanol extract from the aerial parts of F. dibotrys and their structures were identified as benzoic acid (1), p-hydroxybenzoic acid (2), p-hydroxy benzaldehyde (3), 3,4-dihydroxy benzoic acid (4), succinic acid (5), caffeic acid (6), methyl caffeate acid (7), luteolin (8), tricin (9), quercetin (10), afzelin A (11), 2α,3β,29-trihydroxyolean-12-en-28-oic acid (12), yarumic acid (13), and 3α-hydroxy-urs-12,15-dien (14). Conclusion: Compounds 2-3 and 6-9 are firstly obtained from the aerial parts of F. dibotrys. Compounds 11-14 are isolated from the genus of Fagopyrum Mill. for the first time.
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Objective: To study the chemical constituents of Solidago virgaurea and their pharmacological activities. Methods: The compounds were isolated and purified from the plant with chromatography techniques and the chemical structures were identified on the basis of spectrascopic analyses and physicochemical properties, and the anti-inflammatory effects of obtained benzyl benzoate compounds were evaluated by ELISA. Results: Nine compounds were isolated from 90% ethanol extract of S. virgaurea and their structures were identified as 2'-methoxybenzyl-2-methoxy-6-hydroxybenzoate (1), 2'-methoxybenzyl-2, 6-dimethoxybenzoate (2), solidagobenzofuran (3), hexadecanoic acid (4), salicylic acid (5), p-hydroxybenzoic acid (6), solidago virgaurea glycoside (7), kaempferol-3-O-β-D-rutinoside (8), and rutin (9). Conclusion: Compounds 3 and 7 are new compounds; Compounds 4 and 6 are obtained from the plants of Solidago L. for the first time; Compounds 1 and 2 are isolated from this species for the first time. Anti-inflammatory studies show that compounds 1 and 2 could inhibit the TNF-α and IL-6 release of LPS-induced RAW264.7 murine monocytes, while compound 7 shows no significant inhibitory effect.
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Objective: To set up an HPLC method for the simultaneous determination of p-hydroxybenzoic acid plus o-hydroxy-benzoic acid and p-hydroxybenzeneacetic acid in Senecio scandens Buch. Methods:The column was a Shiseido( Fine Chemicals) Cap-cell Pak C18 (250 mm × 4. 6 mm, 5 μm) column at the room temperature. The mobile phase was methanol-water-formic acid (13∶87∶0. 5) at a flow rate of 1. 0 ml·min-1 . The detection wavelength was 240nm. Results: p-Hydroxybenzoic acid plus o-hydroxybenzoic acid had a favorable linear relationship within the range of 0. 025-0. 400 mg·ml-1 , the regression equation was Y=5. 94 × 106 X+2.46×104(r=0.9998),theaveragerecoverywas97.59% andRSDwas1.22%. p-Hydroxybenzeneaceticacidhadafavorableline-ar relationship within the range 0.05-0.80 mg·ml-1, the regression equation was Y=4.09 ×106X+1.12 ×104(r=0.999 8), the average recovery was 98. 07% and RSD was 1. 90%. Conclusion:The method is simple, feasible and reproducible. It can be used in the quality control of p-hydroxybenzoic acid plus o-hydroxybenzoic acid and p-hydroxybenzeneacetic acid in Senecio scandens Buch.