[Determination of organochlorine pesticide residues in the roots of Zanthoxylum nitidum by GC-MS].

OBJECTIVE: To determine the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum and provide scientific foundation for the quality control and standard establishment. METHODS: GC-MS method with selected ion monitoring (SIM) mode was used to analyze the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum. The samples were extracted with acetone and ultrasonic vibrations, and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate -PSA -C18-PestiCarb -phase extraction (SPE) cartridge. RESULTS: Eight kinds of organochlorine pesticide were detected simultanously. Small amounts of OP-DDT were detected in samples 1, 4, 5, 6, 11 and 12, no organochlorine pesticide residue was detected in other samples. The RSD of precision ranged from 0.89% to 2.21%, and the average recovery ranged from 85.33% to 103.70%, with the RSD less than 4%. CONCLUSION: The contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum are less than 0.2 ppm. This method is sensitive, good purifying, and suitable for analyzing organochlorine pesticide residues in the roots of Zanthoxylum nitidum.

[GC-MS analysis of essential oil from Curcuma aromatica rhizome of different growth periods].

OBJECTIVE: To analyze the essential oil from the rhizome of Curcuma aromatica of different growth periods, and to provide the scientific reference for reasonable cultivation and quality control of this plant. METHODS: The essential oil was extracted by hydrodistillation and analyzed with GC-MS. The relative contents were determined with area normalization method. RESULTS: The main volatile constituents in the rhizome of Curcuma aromatica were basically the same. Among these volatile constituents, curdione was the major. The relative content of curdione was 16.35% in the rhizome of wild plant in Hengxian county, and 15.81% in the rhizome of one-year-old plant in Mingyang farm, Nanning city. The relative content of eucalyptol in the 2-year-old cultivated rhizome in Hengxian county was 15.40%, and 14.59% in the rhizome of wild plant in Hengxian county. beta-Elemene, beta-caryophyllene,eugenol and germacrone were also the main constituents in the rhizome essential oil. CONCLUSION: Volatile constituents in the rhizome of Curcuma aromatica are similar to each other,but the relative content of each component is different. This result can provide the scientific foundation for the cultivation of Curcuma aromatica.

[Analysis of compositions of the essential oil from Curcuma aromatica by gas chromatography-mass spectrometry].

OBJECTIVE: To analyze the compositions of the essential oil from the rhizome of Curcuma aromatica in Guangxi. METHODS: The essential oil from the rhizome of Curcuma aromatica was extrated by steam distillation and analysed by GC-MS. RESULTS: 50 chemical constituents accounting for 93.11% of total content were identified. CONCLUSION: The main components are eucalyptol (53.86%), neocurdione (9.89%), linalool (4.24%), camphor (3.14%), alpha-terpineol (2.94%) and germacrone (2.89%).

Structure determination of baeckeins C and D from the roots of Baeckea frutescens.

Baeckeins C (compound 1) and D (compound 2), a pair of new diastereomeric biflavonoids, were isolated from the roots of Baeckea frutescens. Their structures were elucidated on the basis of spectroscopic analysis, including HR-ESI-MS and one- and two-dimensional NMR spectra ((1)H and (13)C NMR, HSQC, HMBC, and ROESY). The absolute configurations of the 2,3-epoxide moiety for compounds 1 and 2 were determined by circular dichroism spectrometry combined with quantum chemical calculations.

Quality evaluation of Potentilla discolor by high-performance liquid chromatography coupled with diode array detection and electrospray ionisation tandem mass spectrometry.

INTRODUCTION: The whole herb of Potentilla discolor has long been used for treatment of diarrhoea, malaria, haemoptysis and haematemesis in clinical applications. However, until now, there has been no literature regarding to the quality control of it. OBJECTIVE: To develop a simple and accurate HPLC-DAD (diode array detection)-ESI/MS(n) (electrospray ionisation multistage mass spectrometry) method for the identification of constituents in P. discolor and simultaneous quantification of its marker compounds. METHODOLOGY: Separations were performed on a Shimpack C18 column by gradient elution using acetonitrile:0.1% formic acid. The identification of constituents in P. discolor were achieved by HPLC-DAD-ESI/MS(n) while six flavonoids and five triterpenoids were determined by HPLC-DAD at 360 and 210 nm, repectively. RESULTS: A total of 23 compounds including 13 flavonoids and 10 triterpenoids were identified or tentatively characterised. A quantitative HPLC-DAD method allowing the simultaneously quantification of 11 marker compounds was optimised and validated for linearity, precision, accuracy, and limits of detection and quantification. The method was successfully applied to the quantification of 11 marker compounds in 10 samples of P. discolor collected from different provinces of China. CONCLUSION: This developed method was validated as simple, precise and accurate, and could be used for effectively and comprehensibly evaluating the quality of P. discolor.

Antidiabetic and antioxidant effects of extracts from Potentilla discolor Bunge on diabetic rats induced by high fat diet and streptozotocin.

AIM OF THE STUDY: Potentilla discolor Bunge, commonly found at the north temperate and boreal zone, has been used for diabetes in China for a long time. Flavonoids and triterpenoids are two major types of compounds in P. discolor. This study was designed primarily to investigate the effects of total flavonoids extract (TFE) and total triterpenoids extract (TTE) of P. discolor Bunge on blood glucose, lipid profiles and antioxidant parameters on diabetic rats induced by high fat diet and streptozotocin. MATERIALS AND METHODS: High fat diet-fed and streptozotocin-induced diabetic rats were treated with the TFE and TTE for 15 days, respectively. A range of parameters were tested including fasting blood glucose (FBG), serum insulin (SI), blood lipid profile, malondialdehyde (MDA), superoxide dismutase (SOD), glutathione (GSH), glycosylated serum protein (GSP), and nitric oxide (NO). RESULTS: Diabetic rats treated with TFE or TTE had decreased concentration of FBG and GSP compared with the control group. Meanwhile, the levels of serum total cholesterol (TC), triglycerides (TG) and low-density lipoprotein cholesterol (LDL-c) in the TFE or TTE treated diabetic rats were lower, and the high-density lipoprotein cholesterol (HDL-c) level was higher than in the control diabetic rats. Furthermore, the extracts treatment decreased the MDA and NO level, while increased SOD and GSH levels in diabetic rats. Histopathologic examination also showed that the extracts have protective effects on ß-cells in diabetic rats which are supported by the increase of SI. CONCLUSIONS: All these experimental results highlighted the hypoglycemic and hypolipidemic properties of the two extracts from Potentilla discolor Bunge on diabetes and its complications, possibly through a strong antioxidant activity and a protective action on ß-cells.

A novel flavanone from Ilex hainanensis Merr.

Chemical investigation of the leaves of Ilex hainanensis Merr. yielded a new flavanone named Huazhongilexone-7-O-beta-D-glucopyranoside, together with five known compounds, which included caffeic acid, quercetin, isoquercitrin, quercitrin-7-O-beta-D-glucopyranoside and rutin. All of the compounds were isolated from the plant for the first time. The structure of the new compound was determined on the basis of high resolution mass, 1D and 2D NMR spectroscopies including ROESY. The antioxidant activity of the new compound was assessed using the DPPH spectrophotometric and IC(50) value was 10.39 micromol L(-1).

[Comparisons of volatile components in different parts of three species of Rhizoma Curcumae].

OBJECTIVE: To provide the scientific basis for the reasonable development and use of the leaves of Rhizoma Curcumae. METHODS: To extract the volatile oil from roots and leaves of three species Rhizoma Curcumae by steam distillation and isolate these products with the method of gas chromatography-mass spectrum. Taking Nist98 standard mass spectrometer database and contrast as control, the structure of the mass spectrogram was identified, and the relative contents of the components were determined with area normalization method. RESULTS: The anti-tumor active constituents such as curdione and germacrone in the leaves had the greater content than in its rhizome. CONCLUSION: The varieties of volatile components in different parts of three species of Rhizoma Curcumae are similar, but their contents are obviously various. We can make the leaves of Rhizoma Curcumae for recycling use.

Complete assignments of 1H and 13C NMR spectral data for three new triterpenoid saponins from Ilex hainanensis Merr.

Three new oleanane-type triterpenoid saponins, ilexhainanoside C, D and E, all with 24, 28-dioic acid groups, were isolated from the leaves of Ilex hainanensis. They were 3beta-hydroxyolean-12-ene-24, 28-dioic acid-28-O-beta-D-glucopyranoside(1), 3beta, 19alpha-dihydroxyolean-12-ene-24, 28-dioic acid-28-O-beta-D-glucopyranoside(2) and 3beta, 29-dihydroxyolean-12-ene-24, 28-dioic acid-28-O-beta-D-glucopyranoside(3). The structures of these three new compounds were elucidated and complete assignments of the (1)H and (13)C NMR spectroscopic data were achieved by 1D and 2D NMR experiments [heteronuclear single quantum coherence (HSQC), HMBC and rotational nuclear Overhauser effect spectroscopy (ROESY)].

Structural determination of two new triterpenoids from Potentilla discolor Bunge by NMR techniques.

Two new pentacyclic triterpenoids, 3alpha, 30-dihydroxylup-20(29)-en-27-oic acid (1) and (20S)-3alpha, 29-dihydroxylupan-27-oic acid (2) were isolated from the whole herbs of Potentilla discolor Bunge. The structures of these two new compounds were elucidated, and complete assignments of the (1)H and (13)C NMR spectroscopic data were achieved by 1D and 2D NMR experiments (HSQC, HMBC, (1)H-(1)HCOSY and ROESY).

Quality assessment of cortex cinnamomi by HPLC chemical fingerprint, principle component analysis and cluster analysis.

HPLC fingerprint analysis, principle component analysis (PCA), and cluster analysis were introduced for quality assessment of Cortex cinnamomi (CC). The fingerprint of CC was developed and validated by analyzing 30 samples of CC from different species and geographic locations. Seventeen chromatographic peaks were selected as characteristic peaks and their relative peak areas (RPA) were calculated for quantitative expression of the HPLC fingerprints. The correlation coefficients of similarity in chromatograms were higher than 0.95 for the same species while much lower than 0.6 for different species. Besides, two principal components (PCs) have been extracted by PCA. PC1 separated Cinnamomum cassia from other species, capturing 56.75% of variance while PC2 contributed for their further separation, capturing 19.08% variance. The scores of the samples showed that the samples could be clustered reasonably into different groups corresponding to different species and different regions. The scores and loading plots together revealed different chemical properties of each group clearly. The cluster analysis confirmed the results of PCA analysis. Therefore, HPLC fingerprint in combination with chemometric techniques provide a very flexible and reliable method for quality assessment of traditional Chinese medicines.

[Study on quality analysis of essential oil from twig and leaf of Baeckea frutescens].

OBJECTIVE: To provide scientific methods for quality criterion by studying the chemical components of essential oil from Baeckea frutescens. METHOD: The chemical components of essential oil from B. frutescens were identified by GC-MS-DS, TLC and capillary GC. The relative contents of main components were determined by area normalization. RESULT: More than 50 peaks were separated, and 38 components were identified, which accounted for over 94% of the total GC peaks areas of the essential oil. The methods for quality evaluation of essential oil from B. frutescens by TLC and capillary GC were established. CONCLUSION: The chemical components of essential oil from B. frutescens collected from different habitats and collecting periods have common characteristics as well as differences. Some components, such as linalool, can be used as a standard and chromatography fingerprint to analyze the quality of essential oil from B. frutescens.