There were significant differences in phenolic acid content between fresh and dried Salvia miltiorrhiza before and after drying. That is to say, the content of phenolic acid in S. miltiorrhiza significantly increased with the increase of dehydration during the drying process.In order to investigate the differences and transformation of free and bound phenolic acids before and after the drying process of S.miltiorrhiza, we studied hydrolysis method, hydrolysates and hydrolysis regularity of phenolic acids in S.miltiorrhiza. UPLC method was used to determine four main hydrolysates of bound phenolic acids, namely danshensu, caffeic acid dimer(SMND-309), caffeic acid, przewalskinic acid A(prolithosperic acid), and three main free phenolic acids in S.miltiorrhiza, namely rosmarinic acid, lithospermic acid, salvianolic acid B. The results of the acid-base hydrolysis experiment of salvianolic acid showed that the alkaline hydrolysis effect was significantly better than acid hydrolysis. The optimal alkaline hydrolysis condition was hydrolysis at 70 ℃ for 4 h with 2 mol·L~(-1) NaOH solution containing 1% ascorbic acid(Vit C). The hydrolysates of free phenolic acids were the same with the hydrolysates of bound phenolic acids. Fresh S.miltiorrhiza contains a low level of free phenolic acids and a high level of bound phenolic acids, which were exactly opposite to dried S.miltiorrhiza. It was suggested that a large amount of bound phenolic acids was accumulated during the growth of S.miltiorrhiza. These bound phenolic acids were coupled with polysaccharides on the cytoderm through ester bonds to form insoluble phenolic acids, which was not easy to be detected by conventional methods. However, during drying and dehydration processes, the bound phenolic acids were converted to a large amount of free phenolic acids under the action of the relevant enzyme.
Desiccation ; Hydroxybenzoates/analysis* ; Salvia miltiorrhiza/chemistry*

To provide a scientific basis for the selection of the appropriate drying method for Mentha Haplocalyx Herba (MHH), determine 2 monoterpenes, 4 phenolic acids and 5 flavonoids in MHH by GC-MS and UPLC-TQ-MS methods, and investigate the effects of the drying methods on the changes in contents of these analytes. The qualities of products obtained with different drying methods were evaluated by the multivariate statistical method of Technique for Order Preference by Similarity to Ideal Solution (TOPSIS). Results showed that the drying methods had the greatest impact on menthol, caffeic acid, and rosemary acid, which were followed by chlorogenic acid and diosmetin-7-O-glucoside. The contents in these analytes processed with hot-air-drying method were higher than those with microwave-drying and infrared-drying methods at the same temperatures. The contents in these analytes processed under low temperature (40-45 °C) were higher than those under higher temperature (60-70 °C). Above all, the contents in phenolic acids processed with microwave fixation (exposed under microwave at 100 °C for several minutes) were obviously higher than those of not being processed, showing an inhibition of some enzymes in samples after fixation. The TOPSIS evaluation showed that the variable temperature drying method of 'Hot-Air 45-60 °C' was the most suitable approach for the primary drying processing of MHH. The results could provide the scientific basis for the selection of appropriate drying method for MHH, and helpful reference for the primary drying proces of herbs containing volatile chemical components.
Desiccation ; methods ; Flavonoids ; analysis ; Hydroxybenzoates ; analysis ; Mentha ; chemistry ; Monoterpenes ; analysis

OBJECTIVETo establish the fingerprint chromatograms of the extract of Cimicifugae Rhizoma firstly.

METHODPhenolic acids and triterpenoid saponins were analyzed by HPLC. Hypersil BDS C18 (4.6 mm x 250 mm, 5 microm) column was used, the mobile phase was composed of acetonitrile -0.1% H3PO4 with gradient elution, flow rate was 1.0 mL x min(-1), column temprature was 30 degrees C, and the detection wavelength was set at 316 nm and 210 nm.

RESULTIn the fingerprint of phenolic acids, thirteen feature peaks were found and the RSD of relative retention time and relative peak area were all less than 3% in the precision and repeation experiments. The similarity of ten batches of samples were all more than 0.90. In the fingerprint of triterpenoid saponins, fourteen feature peaks were found and the RSD of relative retention time and relative peak area were all less than 4% in the precision and repeation experiments. The similarity of ten batches of samples were all more than 0.90.

CONCLUSIONThis method is comprehensive, stable, reliable and can be used to evaluate the quality of the extract of Cimicifugae Rhizoma. It has provided a reference to the analysis on pharmacodynamic deferences of Cimicifuga extracts and also laid the foundation for its further development.

Chromatography, High Pressure Liquid ; methods ; Cimicifuga ; chemistry ; Hydroxybenzoates ; analysis ; Plant Extracts ; analysis ; Saponins ; analysis ; Triterpenes ; analysis

To study the non-flavonoids chemical constituents in water extract of Spatholobi Caulis. Some purification and analysis techniques like silica gel, D101-macroporous adsorptive resins, and Sephadex LH-20 column chromatographies as well as reversed phase high-performance liquid chromatography were used to isolate and analyze the phenolic acid esters and other type compounds from Spatholobi Caulis integrally. The structures of these compounds were identified by spectroscopic techniques such as nuclear magnetic resonance and high resolution mass spectrometries. Twenty-seven compounds, including phenolic acid, coumarin, lignan, terpene, alkaloid, and steroid compounds, were isolated from ethyl acetate and n-butanol fractions in water extract of Spatholobi Caulis, and they were identified as β-sitosterol(1), feruli acid methyl ester(2), syringaresinol(3),(+)-medioresinol(4),(+)-epipinoresinol(5), p-acetylphenol(6), bolusanthin Ⅳ(7), evofolin B(8), salicylic acid(9), trans-p-hydroxy-cinnamic acid(10), abscisic acid(11), m-hydroxyphenol(12), C-veratroylglycol(13), p-hydroquinone(14), 8,9-dihydroxymegastigma-4,6-dien-3-one(15), p-hydroxybenzoic acid(16), 6,9-dihydroxymegastigma-4,7-dien-3-one(17), protocatechuic acid(18), protocatechuic acid methyl ester(19), 5,7-dihydroxycoumarin(20), isolariciresinol(21), nicotinic acid(22), daucosterol(23),(+)-pinoresinol(24), stigmasterol(25), allantoin(26) and koaburaside(27), respectively. Furthermore, compounds 2-15, 19-22, 24 and 26 were isolated from genus Spatholobus for the first time.
Drugs, Chinese Herbal/analysis* ; Esters/analysis* ; Fabaceae/chemistry* ; Hydroxybenzoates/analysis* ; Mass Spectrometry ; Phytochemicals/analysis*

Eighteen compounds were isolated by a combination of various chromatographic techniques including column chromatography over macroporous resin, MCI gel, silica gel, and sephadex LH-20 and reversed-phase HPLC. Their structures were elucidated by spectroscopic data analysis as adinoside A (1), stryspinoside (2), benzyl alcohol beta-glucopyranoside (3), benzyl 2-o-beta-D-glucopyranosyl-2,6-dihydroxybenzoate (4) , gentisic acid 2-O-beta-D-glucopyranoside (5), eugenyl beta-D-glucopyranoside (6) , eugenyl-P-xylopyranosyl-(1-->6)-beta-glucopyranoside (7), (-)-lyoniresinol 9-O-fP-D-glucopyranoside (8) , (+)-lyoniresinol 9-O-beta-D-glucopyranoside (9) , apigenin-7-O-L-rhamnopyranoside (10), luteolin-3 '-O-L-rhamnoside (11) , ursolic acid (12) , beta-sitosteryl-3beta-glucopyranoside-6'-O-palmitate (13), abscisic acid (14), guanosine (15), 5-methyluracil (16), trans-cinnamic acid (17), and 4-hydroxybenzaldehyde(18). These compounds were obtained from this plant for the first time.
Benzaldehydes ; analysis ; Flowers ; chemistry ; Gentisates ; analysis ; Glucosides ; analysis ; Hydroxybenzoates ; analysis ; Lonicera ; chemistry ; Luteolin ; analysis ; Thymine ; analysis ; Triterpenes ; analysis

This paper was aim to determine five phenolic acids, sodium danshensu (SD), protocatechuic aldehyde (PA), rosmarinic acid (RA), lithospermic acid (LA) and salvianolic acid B (SAB), in Guanxinning injection. In the test, Kromasil C18 column (4.6 mm x 250 mm, 5 µm) was adopted, with acetonitrile-3% formic acid solution as the mobile phase for gradient elution. The flow rate was 1 mL · min, the column temperature was 30 °C and the detection wavelength was 280 nm. According to the results of the test, SD, PA, RA, LA and SAB showed good linear relations between peak areas and sample sizes in 0.006 06-4.04 (r = 0.999 3), 0.006 15-4.10 (r = 0.999 4), 0.005 94-3.96 (r = 0.999 3), 0.006 06-4.04(r = 0.999 1) and 0.006 09-4.06 (r = 0.999 2) µg, respectively. The average recoveries (n = 6) were 98.9% (RSD 0.75%), 98.1% (RSD 1.2%), 100% (RSD 0.77%), 98.7% (RSD 1.7%), 102% (RSD 0.68%), respectively. The above 5 components were determined in 13 batches of samples by using the established method. The method was simple, accurate and highly reproducible that it could be used for quality control of the components in Guanxinning injection.
Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; Hydroxybenzoates ; analysis

OBJECTIVETo investigate the AAPH scavenging activities of 22 flavonoids and phenolic acids and 9 extracts of Chinese materia medica.

METHODThe antioxidant activities of the samples were evaluated by an oxygen radical absorbance capacity method (ORAC), at the same time, the total contents of flavonoids and phenolic the 9 herb extracts were analyzed by Folin-Ciocalteu method, and the active components were qualitatively and quantitatively analyzed by an HPLC method.

RESULTIt was found that the tea extract showed the strongest AAPH activity with the ORAC value of 4786.40 micromol x g(-1) whereas safflower demonstrated the weakest activity with the ORAC value of 784.04 micromol x g(-1). As for compounds, quercetin had the strongest AAPH activity with the ORAC value of 12.90 while ( - )-EGC had the weakest activity with the ORAC value of 2.47. A quantitative relationship was obtained to describe the AAPH scavenging activity of the herb extracts: Y = 1844.8 lnX-3577.5, r = 0.8675, where Y stands for the ORAC vaule, and X stands for the concentration of total phenolic acids.

CONCLUSIONFlavonoids and phenolic acids are the AAPH scavenging active ingredients in the Chinese herb extracts. It's a good way to study the antioxidant activity of Chinese herb extract and its chemical composition by combing ORAC method and HPLC method.

Amidines ; analysis ; Drugs, Chinese Herbal ; analysis ; Flavonoids ; analysis ; Free Radical Scavengers ; analysis ; Hydroxybenzoates ; analysis ; Materia Medica ; chemistry ; Plants, Medicinal ; chemistry

To investigate the chemical constituents from Commelina communis, fifteen compounds were separated and purified by silica gel, Sephadex LH-20, and ODS column chromatography, and semi-preparative HPLC. By analyses of NMR and MS data as well as their physical and chemical properties, the structures of these compounds were identified as chrysoeriol-7-O-beta-D-glucoside( 1), methyl gallate(2), p-coumaric acid(3), protocatechuic acid(4), caffeic acid(5), p-hydroxybenzoic acid(6), 2-phenethyl-beta-D-gly-cosidase(7) , rhaponticin(8) , (7S, 8R) -dihydrodehydrodiconiferyl alcohol-9-O-beta-D-glucoside (9), isovitexin (10) , isofurcatain (11), isorhamnetin-3-O-beta-D-glucoside(12) , quercetin-3-O-alpha-L-rhamnoside (13) , isoquercitrin (14) , and 1, 2-dihydro-6, 8-dime-thoxy-7-1-(3, 5-dimethoxy-4-hydroxyphenyl) -N1, N2-bis-[2-( 4-hydroxyphenyl) ethyl] -2, 3-naphthalene dicarboxamide (15). Compounds 2, 5-9, 11, 13 were obtained from the genus Commelina for the first time.
Caffeic Acids ; analysis ; Chromatography, High Pressure Liquid ; Commelina ; chemistry ; Glucosides ; analysis ; Hydroxybenzoates ; analysis ; Quercetin ; analogs & derivatives ; analysis

OBJECTIVETo establish a RP-HPLC method for the determination of four acids compounds including gallic acid, protocatechuic acid, corilagin and ellagic acid in Erodium Stephanianum.

METHODThe RP-HPLC separation was performed on an Agilent TC-C18 analytical column (4.6 mm x 250 mm, 5 microm). The mobile phase was methanol (A) -water containing 0.4% H3PO4 (B) with gradient elution mode at the flow rate of 0.8 mL x min(-1). The detection wavelength was set at 259 nm, and the column temperature was 30 degrees C.

RESULTThe liner ranges of gallic acid, protocatechuic acid, corilagin and ellagic acid were 0.059-2.360 g x L(-1) (r = 0.999 6), 0.017-0.672 g x L(-1) (r = 0.999 9), 0.351-14.040 g x L(-1) (r = 0.999 9), and 0.151-6.040 g x L(-1) (r = 0.999 8), respectively. The average recoveries (n = 3) were 99.45% (RSD 1.5%), 98.65% (RSD 1.7%), 100.3% (RSD 2.0%), and 98.90% (RSD 1.2%), respectively.

CONCLUSIONThe method is simple and accurate with a good reproducibility and can be used for quality control of Erodium stephanianum.

Chromatography, High Pressure Liquid ; methods ; Ellagic Acid ; analysis ; Gallic Acid ; analysis ; Geraniaceae ; chemistry ; Glucosides ; analysis ; Hydrolyzable Tannins ; Hydroxybenzoates ; analysis

OBJECTIVETo study the variation Laws of content of danshensu accelerated in control and in danshen injection in order to provide reference for stability investigation of danshensu.

METHODThe tests was carried out by classic isothermal method and the content of danshensu was determined by HPLC.

RESULTThe contents of danshensu in accelerated tests increase in control and decrease in danshen injection respectively.

CONCLUSIONThe component of phenic acidity would be hydrolyzed to become danshensu in the accelerated tests. Much attention should be paid to the unusual increase when studies of danshen preparations are carried out.

Chromatography, High Pressure Liquid ; Drug Stability ; Hydrolysis ; Hydroxybenzoates ; chemistry ; Injections ; Lactates ; administration & dosage ; analysis ; chemistry ; Temperature