OBJECTIVETo compare the contents of iridoid among the fruit, seed, and pericarp from Gardenia jasminoides.

METHODThe contents of geniposide and genipin gentiobioside were determined simultaneously by HPLC. A Kromasil C18 column at 35 degrees C was used with the acetonitrile-0.3% formic acid anhydrous (12: 88) as the mobile phases. The detection wavelength was set at 238 nm and the flow rate was 1.0 mL x min(-1).

RESULTThe obtained linearity of the two components was better over 0.999 4 and the average recoveries were 99.11%, 98.47%, respectively. The results exhibited the remarkable variation among the different parts of the fruit.

CONCLUSIONThe contents of the two constituents in seed were higher than in pericarp.

Fruit ; chemistry ; Gardenia ; chemistry ; Iridoids ; analysis ; Seeds ; chemistry

OBJECTIVETo develop an HPLC method for determination of loganin in Pterocephalus hookeri.

METHODThe analysis was performed on a Welchrom C18 column (4.6 mm x 250 mm, 5 microm) with acetonitrile-water (12:88) as the the mobile phase at a flow rate of 1 mL x min(-1) and the detection wavelength was 240 nm.

RESULTThe peak areas and injection amounts of loganin had a good linear relationship at the range of 0.06-1.2 microg. The average recovery was 97.0%, and the RSD was 1.4%.

CONCLUSIONThe method is simple, accurate, and can be used for its quality control.

Chromatography, High Pressure Liquid ; methods ; Iridoids ; analysis ; Medicine, Tibetan Traditional ; Plants, Medicinal ; chemistry

OBJECTIVETo compare the contents of the main chemical compositions in Gardenia jasminoids before and after being roasted with ginger juice.

METHODFour diterpenoid pigments constituents (C-1, C-2, C-3, crocetin) were determined simultaneously by UPLC on an Agilent Poroshell 120 EC-C18 column at 35 degrees C with the methanol-0.5% formic acid anhydrous in gradient elution as the mobile phrase. The detection wavelength was set at 440 nm and the flow rate was 0.4 mL x min(-1). Two iridoids constituents (G-1, G-2) were determined simultaneously by HPLC on an Agilent TC-C18(2) column at 35 degrees C with acetonitrile-0.5% formic acid anhydrous (18:82) as the mobile phrase. The detection wavelength was set at 238 nm and the flow rate was 1.0 mL x min(-1).

RESULTAfter being processed with ginger juice, the contents of the diterpenoid pigments constituents decreased slightly and the contents of the iridoids constituents increased slightly.

CONCLUSIONThe contents of the main chemical compositions in G. jasminoids roasted with ginger juice increased slightly with some regularity, but there were no significant differences.

Carotenoids ; analysis ; Chemistry, Pharmaceutical ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; analysis ; Gardenia ; chemistry ; Ginger ; chemistry ; Iridoids ; analysis ; Pharmacology

Application of a combination of various chromatographic techniques including column chromatography over silica gel, Sephadex LH-20, macroporous adsorbent resin, and reversed-phase HPLC, led to the isolation of 173 compounds including irdidoids, monoterpenes, sesquiterpenes, triterpenes, lignans, flavonoids, and simple aromatic derivatives from the ethyl acetate-soluble fraction of the whole plants of Valeriana jatamansi(Valerianaceae), and their structures were elucidated by spectroscopic methods including 1D, 2D NMR UV, IR, and MS techniques. Among them, 77 compounds were new. In previous reports, we have described the isolation, structure elucidation, and bioactivities of 68 new and 25 known compounds. As a consequence, we herein reported the isolation and structure elucidation of the remaining 9 new and 71 known compounds, the structure revision of valeriotriate A(8a), as well as cytotoxicity of some compounds.
Acetates ; Chromatography, High Pressure Liquid ; Flavonoids ; analysis ; Iridoids ; analysis ; Lignans ; analysis ; Molecular Structure ; Monoterpenes ; analysis ; Phytochemicals ; analysis ; Plant Extracts ; chemistry ; Sesquiterpenes ; analysis ; Triterpenes ; analysis ; Valerian ; chemistry

OBJECTIVETo develop an HPLC method for the determination of oleuropein in Syringa oblata.

METHODAn Aigilent ZORBAX SB- C18 column (4.6 mm x 250 mm, 5 microm) was used. The mobile phase was acetonitrile-water (21 : 79). The flow rate was 1.0 mL x min(-1). The detection wavelenghth was set at 232 nm and the column temperature was 30 degrees C.

RESULTThe linear range of oleuropein were from 0.011 62 g x L(-1) to 1.162 g x L(-1). The average recovery was 98.7% with RSD 2.5% (n=9).

CONCLUSIONThe method is reliable, accurate and specific. It can be used for quality control of the stem of Syringa oblata.

Acetonitriles ; chemistry ; Benzoates ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; Iridoids ; Pyrans ; analysis ; Syringa ; chemistry ; Vasodilator Agents ; analysis

OBJECTIVETo study the chemical constituents of the roots of Phlomis medicinalis.

METHODThe compounds were isolated and repeatedly purified by macroporous resin, silica gel column chromatography, TLC and PREP-HPLC. Their structures were elucidated by physical and chemical properties and NMR spectra.

RESULTTwo iridoid glucosides were obtained and elucidated as 7-epilamalbide (1), chlorotuberoside (2).

CONCLUSIONCompound 1 was a new compound, compound 2 was isolated from the plant for the first time.

Glucosides ; analysis ; isolation & purification ; Iridoid Glucosides ; Iridoids ; analysis ; isolation & purification ; Magnetic Resonance Spectroscopy ; Phlomis ; chemistry ; Plant Roots ; chemistry

To establish the high performance liquid chromatography (HPLC) fingerprint for Digeda-4 decoction (DGD-4D), determine the contents of aesculetin, geniposide, picroside Ⅰ, picroside Ⅱ and ellagicacid in DGD-4D, and provide the scientific foundation for quality control of DGD-4D. The analysis was performed on Diamonsil(2) C₁₈ (4.6 mm×250 mm,5 μm) column, with methanol-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution. The flow rate was 1.0 mL·min⁻¹; injection size was 10 μL; temperature was maintained at 30 °C, and the detection wavelength was set at 254 nm. The common mode of DGD-4D HPLC fingerprint was established, and the hidden information was analyzed by Chemometrics. Chromatographic peaks for DGD-4D were identified by HPLC and quantitative analysis was conducted for characteristic peaks. There were 17 common peaks in the fingerprints and the similarity of the fingerprints was over 0.9 in all 15 batches. The samples were broadly divided into four kinds by principal component analysis and clustering analysis. Four marker compounds were verified by partial least squares discriminant analysis, and No. 9, 12 and 14 peaks were identified as geniposide, picroside Ⅱ, and picroside Ⅰ respectively. The average recoveries were in the range of 95.91%-97.31%. The HPLC fingerprint method for content determination is reliable, accurate, rapid, simple, and reproducible, and can be used as one of the effective methods to control the quality of DGD-4D.
Chromatography, High Pressure Liquid ; Cinnamates ; Drugs, Chinese Herbal ; analysis ; standards ; Iridoid Glucosides ; Iridoids ; Methanol ; Principal Component Analysis ; Quality Control

OBJECTIVETo develop an HPLC method for the quantification of six active components in three species (Swertia davidi, S. nervosa and S. mussotii) .

METHODThe determination was performed on a Hypersil BDS colunm (4. 6 mm x 200 mm, 5 microm). Acetonitrile and 0.5% phosphoric acid solution were used as the mobile phases with a gradient elution. The flow rate was 1.0 mL x min(-1). The UV detection wavelength was at 240, 274, 325 and 334 nm. The column oven temperature was at 25 degrees C.

RESULTSix components were separated commendably in 60 minutes. The calibration curves of swertiamarin, gentiopicroside, norswertianolin, swertianolin, demethylbellidifolin and bellidifolin were in good linearity over the range of 0.520-20.8, 0.202-8.06, 0.107-4.28, 0.097-3.86, 0.094-3.77, 0.101-4.02 microg, respectively (r = 0.999 9). The average recoveries were 98.7%, 98.1%, 98.3%, 98.8%, 98.1% and 98.6%, respectively, and the RSD were less than 3.0% (n = 6).

CONCLUSIONThe method is accurate,simple and reproducible, and can be used to control the quality of Swertia.

Chromatography, High Pressure Liquid ; instrumentation ; methods ; Drugs, Chinese Herbal ; analysis ; Glucosides ; analysis ; Iridoid Glucosides ; Iridoids ; analysis ; Pyrones ; analysis ; Swertia ; chemistry ; Xanthones ; analysis

This study aimed to explore the correlation of the content of 15 non-crocin components of Gardeniae Fructus with its external properties(shape and color). The fruit shape was quantified according to the length/diameter measured by ruler and vernier calliper and the chromaticity values L~*, a~*, b~*, and ΔE~* of all samples were determined by chroma meter. Chromatographic separation was conducted on a Welch Ultimate XB C_(18) column(4.6 mm×250 mm, 5 μm) under gradient elution with acetonitrile solution(A) and 0.1% formic acid aqueous solution(B) as the mobile phase at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃ and the detection wavelength was 238 nm. The high-performance liquid chromatography(HPLC) method was established for simultaneous determination of the content of eight iridoid glycosides, six phenolic acids, and one flavonoid in 21 batches of Gardeniae Fructus samples. The correlation of the content of the 15 components with shapes and chromaticity values in each sample was analyzed by multivariate statistical analysis. According to the circulation situation and traditional experience, 21 batches of Gardeniae Fructus samples were divided into three categories, namely 14 batches of Jiangxi products(small and round, red and yellow), 4 batches of Fujian products(oval, red) and 3 batches of Shuizhizi(Gardenia jasminoides, longest, reddest). The Gardeniae Fructus samples were sequenced as Jiangxi products(1.71) < Fujian products(1.99) < Shuizhizi(2.55) in terms of the length/diameter average, Jiangxi products(17.7) < Fujian products(19.7) ≈ Shuizhizi(19.6) in terms of average value of a~*(red and green), Jiangxi products(24.4) > Fujian products(19.2) ≈ Shuizhizi(19.3) in terms of b~*(yellow and blue), and Jiangxi products(49.8) > Fujian products(48.0) ≈ Shuizhizi(47.8) in terms of L~*(brightness). The total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Jiangxi products was in the ranges of 65.53-99.64, 52.15-89.16, 6.10-11.83, and 0.145-1.81 mg·g~(-1), respectively. The total amount of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Fujian products was in the ranges of 69.33-94.35, 63.52-85.19, 5.39-8.41, and 0.333-0.757 mg·g~(-1), respectively. In Shuizhizi, the total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin was in the ranges of 77.35-85.98, 68.69-76.56, 7.30-9.05, and 0.368-0.697 mg·g~(-1), respectively. Pearson correlation analysis revealed that Gardeniae Fructus with leaner and longer fruit shape possessed lower content of total phenolic acids(the sum of the six phenolic acids) and rutin, but the correlation with iridoid glycosides was not high. Additionally, the higher content of total phenolic acids and rutin denoted the yellow coloration of Gardeniae Fructus, and the higher content of cryptochlorogenic acid, chlorogenic acid, and rutin meant the brighter color of Gardeniae Fructus. However, the higher content of geniposide and neochlorogenic acid and the lower content of deacetyl asperulosidic acid methyl ester led to the red coloration of Gardeniae Fructus. The results indicated that the morphological characters of Gardeniae Fructus were closely related to its chemical components. The more round shape and the yellower color reflected the higher content of phenolic acids and flavonoid, and Gardeniae Fructus with redder color had higher content of geniposide. OPLA-DA showed that the length/diameter and the content of six iridoid glycosides(gardoside, shanzhiside, gardenoside, genipin 1-gentiobioside, 6β-hydroxy geniposide, and deacetyl asperulosidic acid methyl ester), two phenolic acids(neochlorogenic acid and cryptochlorogenic acid) and rutin could be used as markers to distinguish three types of samples. This study provided experimental data for the scientific connotation of "quality evaluation through morphological identification" of Gardeniae Fructus.
Chromatography, High Pressure Liquid/methods* ; Drugs, Chinese Herbal/analysis* ; Esters/analysis* ; Flavonoids/analysis* ; Fruit/chemistry* ; Gardenia/chemistry* ; Iridoids/analysis* ; Rutin/analysis*

OBJECTIVEA new method for the simultaneous quantitative determination of geniposide, baicalin and berberine hydrochloride in Angong Niuhuang pill using reversed phase high performance liquid chromatographic method had been developed.

METHODThe optimum chromatographic conditions were as follows: Agilent Zorbax SB - C18 column (4.6 mm 250 mm, 5 m), acetonitrile-H2O (containing 6 mmol L(-1) KH2PO4, pH 4.6) gradient elution; as a detection wavelength of 343 nm.

RESULTThe calibration curves of geniposide, baicalin and berberine were linear at the ranges of 4.50-110.00, 5.00-153.00, 6.40-191.00 mg L(-1), respectively. The limits of detection of the method were 0.77 ng for geniposide, 1.53 ng for baicalin and 1.43 ng for berberine hydrochloride. The recoveries of the method were 104.44% (RSD 1.79% ) for geniposide, 96.98% (RSD 1.76%) for baicalin, 101.08% (RSD 3.1%) for berberine hydrochloride.

CONCLUSIONThis method had been successfully applied to determine the content of geniposide, baicalin and berberine hydrochloride in Angong Niuhuang pill.

Berberine ; analysis ; Chromatography, High Pressure Liquid ; methods ; Drug Combinations ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Flavonoids ; analysis ; Iridoids ; analysis ; Materia Medica ; chemistry ; Plants, Medicinal ; chemistry ; Pyrans ; analysis