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1.
China Pharmacy ; (12): 1220-1224, 2022.
Article in Chinese | WPRIM | ID: wpr-924075

ABSTRACT

OBJECTIVE To establish a met hod for the determination of amentoflavone ,bilobetin,ginkgetin,isoginkgetin and sciadopitysin in Ginkgo biloba leaves tablets. METHODS After extracted with methanol ,ultra-performance liquid chromatography (UPLC)was adopted to determine G. biloba leaves tablets. The determination was performed on Waters Acquity UPLC HSS T 3 column with acetonitrile- 0.4% phosphoric acid as mobile phase (gradient elution )at the flow rate of 0.4 mL/min. The column temperature was set at 35 ℃,and the detection wavelength was 340 nm. The sample size were 1 μL(substance control )and 10 μL (test sample ). The relative correction factors (RCFs)of bilobetin ,ginkgetin,isoginkgetin and sciadopitysin were calculated by quantitative analysis of multicomponents by single marker (QAMS)using amentoflavone as control. The chromatographic peak was located with the relative retention time method. Then the contents of the above components were calculated ,and the results were compared with those of external standard method (ESM)(except for amentoflavone ). RESULTS The linear ranges of amentoflavone,bilobetin,ginkgetin,isoginkgetin and sciadopitysin were 0.10-8.21,0.24-19.34,0.16-12.98,0.22-17.66,0.06-4.86 ng,respectively(all r>0.999). The quantitation limits were 0.10,0.24,0.16,0.22,0.06 ng,respectively. RSDs of precision , repeatability and stability tests (36 h)were all lower than 3.00%. The average recoveries were 99.77%-102.85%,and RSDs were 1.90%-4.40%(n=6). The average RCFs of bilobetin ,ginkgetin,isoginkgetin and sciadopitysin were 0.91,0.93,0.96 and 0.95, respectively. The average relative retention times were 1.08,1.18,1.19 and 1.30,respectively. The relative deviation between the calculation result of QAMS and ESM was within ±3.00%. CONCLUSIONS The established method is accurate and stable ,and can be applied to the determination of Ginkgo biflavones in G. biloba leaves tablets and control the quality.

2.
Article in Chinese | WPRIM | ID: wpr-905908

ABSTRACT

Objective:To establish ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for simultaneous determination of six hepatotoxic pyrrolizidine alkaloids in Verbenae Herba, and to carry out preliminary risk assessment according to the research results. Method:An ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm) was used for analysis with 0.05% formic acid and 2.5 mmol·L<sup>-1</sup> ammonium formate in water (A)-0.05% formic acid and 2.5 mmol·L<sup>-1</sup> ammonium formate in acetonitrile (B) as mobile phase for gradient elution (0-12 min, 3%-8%B; 12-25 min, 8%-15%B; 25-26 min, 15%-3%B; 26-30 min, 3%B), the flow rate was 0.3 mL·min<sup>-1</sup>, the column temperature was 40 ℃, and the injection volume was 1 μL. MS system was operated by electrospray ionization (ESI) in the positive ion mode with multiple reaction monitoring mode. MS parameters of triple quadrupole and six analytes were optimized for qualitative and quantitative analysis. According to the determination results, the risk assessment was carried out by using margin of exposure (MOE) combined with transfer rate of hot water extraction. Result:Based on the instrument precision, linear range, repeatability, stability, recovery and other methodological validations, the results were in conformity with relevant standards of quantitative analysis. The linear ranges of intermedine, lycopsamine, intermedine <italic>N</italic>-oxide, lycopsamine<italic> N</italic>-oxide, echimidine<italic> N</italic>-oxide and echimidine were good (<italic>r</italic>≥0.999 0) between peak area and mass concentration in the ranges of 0.984-49.20, 0.994-49.70, 1.012-50.60, 1.032-51.60, 1.004-50.20, 1.016-50.80 µg·L<sup>-1</sup>, respectively. The average recoveries of these six analytes were 87.2%-94.2% with relative standard deviation (RSD)<4.0%. Their MOE values were >10 000. Conclusion:The UPLC-MS/MS established in this study is stable and feasible, which can provide scientific basis for the quality control and safety evaluation of hepatotoxic pyrrolizidine alkaloids in Verbenae Herba.

3.
Article in Chinese | WPRIM | ID: wpr-905076

ABSTRACT

Objective:To conduct quality evaluation of Ginkgo Folium preparations by analyzing the national evaluation sampling test results, analyze the quality differences, and put forward suggestions for the improvement of quality standards and market supervision. Method:The contents of total flavonol glycosides and terpene lactones in Ginkgo Folium tablets and Ginkgo Folium capsules were determined according to the methods of determination in the 2015 edition of Chinese Pharmacopoeia (the first volume), and the contents of free flavonoids (quercetin, kaempferide and isorhamnetin) and sophoricoside in Ginkgo Folium preparations were determined according to related supplementary testing method of Ginkgo Folium tablets and Ginkgo Folium capsules issued by National Medical Products Administration. The quality differences of Ginkgo Folium preparations from different batches and different manufacturers were compared according to the contents of total flavonol glycosides, terpene lactones, free flavonoids and sophoricoside in 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules manufactured by 48 enterprises. Result:Quality of 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules was in accordance with the standard, but the contents of terpene lactones and total flavonol glycosides were all distributed in a wide range, and the quality of samples varied greatly among different enterprises. Conclusion:It is recommended that each enterprise should optimize the production process and strictly control the raw materials to ensure the consistency between different batches of samples.

4.
Article in Chinese | WPRIM | ID: wpr-921642

ABSTRACT

This study intends to develop a high performance liquid chromatography-diode array detection(HPLC-DAD) method for simultaneous determination of chlorogenic acid, 2-hydroxymethyl-3-hydroxyl-1-butene-4-O-β-D-(6″-O-caffeoyl)-glucopyranoside, pubescenoside B, huazhongilexone-7-O-β-D-glucopyranoside, rutin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C in Ilex hainanensis. The HPLC conditions are as follows: Waters XBridge C_(18 )column(4.6 mm×250 mm, 5 μm), mobile phase of 0.5% formic acid in water(A)-acetonitrile(B), gradient elution(0-8 min, 5%-12% B; 8-18 min, 12%-18% B; 18-30 min, 18%-25% B; 30-40 min, 25%-30% B; 40-42 min, 30%-80% B; 42-45 min, 80% B) at the flow rate of 0.8 mL·min~(-1), detection wavelengths of 282, 324, and 360 nm, column temperature of 25 ℃, and injection volume of 5 μL. The content of the 8 phenols in 8 samples was 0.30-6.29, 0.29-3.27, 0.15-10.4, 0.51-5.85, 0.49-9.02, 0.51-4.68, 1.93-13.4, and 0.87-5.95 mg·g~(-1), respectively. Moreover, the content of phenols in the samples collected in October was higher than that of samples harvested in other months. The established method is accurate and sensitive for the determination of phenols in I. hainanensis, which is useful for the quality improvement of this herbal medicine.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Ilex , Phenols
5.
Article in Chinese | WPRIM | ID: wpr-888146

ABSTRACT

This study aims to develop a UPLC-MS/MS method for simultaneous determination of six pyrrolizidine alkaloids(PAs)--intermedine N-oxide(ImNO), lycopsamine N-oxide(LyNO), seneciphylline(Sp), seneciphylline N-oxide(SpNO), senecionine N-oxide(SnNO), and senkirkine(Sk) in different parts of Emilia sonchifolia. UPLC conditions are as follows: ACQUITY UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm), mobile phase consisting of 0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in water(A)-0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in acetonitrile(B) for gradient elution. MS conditions are as below: electrospray ionization(ESI) in the positive ion mode, multiple reaction monitoring(MRM), and the content of the six PAs was calculated with the external standard method. The results suggested the differences in the six PAs among different parts of E. sonchifolia. Sk was detected in all the four parts, with similar content. SnNO also existed in all the four parts, but the content in roots was significantly higher than that in other parts. Sp and SpNO were found in both roots and flowers, with the content higher in the former than in the later. ImNO and LyNO were only found in leaves, and the content was low. Among the six components detected, ImNO, LyNO, and SpNO were found and determined for the first time, which enriched the toxic components and laid a scientific basis for the quality and safety evaluation of E. sonchifolia.


Subject(s)
Asteraceae , Chromatography, High Pressure Liquid , Chromatography, Liquid , Pyrrolizidine Alkaloids , Tandem Mass Spectrometry
6.
Article in Chinese | WPRIM | ID: wpr-827970

ABSTRACT

This study aims to establish an HPLC method for the simultaneous determination of 6 main components, including chlorogenic acid, 3,4-dicaffeoylquinic acid,3,5-dicaffeoylquinic acid,4,5-dicaffeoylquinic acid, pellitorine and neopellitorine B in Achil-leae Herba. HPLC analysis was performed on a Merck Purospher STAR RP-18 endcapped(4.6 mm×250 mm, 5 μm), with a mobile phase consisting of 0.05% phosphoric acid solution(A)-acetonitrile(B) at a flow rate of 1 mL·min~(-1)(0-7 min,12%-14% B;7-10 min,14%-17% B;10-25 min,17%-22% B;25-35 min,22%-35% B;35-51 min,35%-80% B;51-60 min,80%-90% B). The detection wavelength was 254 nm and the column temperature maintained at 30 ℃, and the injection volume was 5 μL. The standard curves revealed a good linear relationship. The contents of 6 components were 0.404%-2.116% for chlorogenic acid, 0.160%-0.892% for 3,4-dicaffeoylquinic acid, 0.608%-1.464% for 3,5-dicaffeoylquinic acid, 0.168%-0.868% for 4,5-dicaffeoylquinic acid, 0.122%-1.234% for pellitorine, 0.065%-0.312% for neopellitorine B, respectively. Both cluster and principal component analysis can distinguish the research data in anthesis and pre-anthesis by software Chempattern. There were obviously differences in the different harvest time. Therefore, attention should be paid to the harvesting time of the herb. The method can be used to determine the contents of six main components, and can provide reference for the improvement of quality standard of Achilleae Herba.


Subject(s)
Chlorogenic Acid , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Principal Component Analysis
7.
Article in Chinese | WPRIM | ID: wpr-773656

ABSTRACT

Based on UPLC specific chromatogram and determination of seven main components,this study aimed at evaluating the quality of Cistanche deserticola,C. tubulosa and C. sinensis. Echinacoside,cistanoside A,verbascoside,tubuloside A,isoacteoside,2'-acetylacteoside,tubuloside B were used as reference substances. UPLC analysis was performed on a Waters ACQUITY UPLC HSS T3 column( 2. 1 mm×100 mm,1. 8 μm). The mobile phase was acetonitrile-0. 08% trifluoroacetic acid solution. The flow rate was0. 3 mL·min-1,and the injection amount was 10 μL. The column temperature was 40 ℃,and the detection wavelength was 330 nm.The UPLC specific chromatograms were processed with ChemPattern software. UPLC specific chromatograms of C. deserticola and C.tubulosa from different samples were of high similarity,but the similarities of their counterfeit C. sinensis were less than 0. 06. Both of cluster and principal component analysis can distinguish certified products and counterfeits. The content ratios of echinacoside/verbascoside and verbascoside/isoacteoside were quite different between C. deserticola and C. tubulosa,which had distinct significance.The UPLC specific chromatogram and contents of seven main components can provide a basis for quality evaluation of Cistanches Herba.


Subject(s)
Chromatography, High Pressure Liquid , Cistanche , Chemistry , Classification , Drugs, Chinese Herbal , Reference Standards , Phytochemicals , Principal Component Analysis
8.
Article in Chinese | WPRIM | ID: wpr-773140

ABSTRACT

The aim of this paper was to compare the influence of freeze-drying and sun-drying on six main nucleosides and nucleobases of Cordyceps sinensis by HPLC. Hypoxanthine,xanthine,uridine,inosine,guanosine and adenosine were reference substances. HPLC analysis was performed on a GL Inertsustain AQ-C_(18) column( 4. 6 mm×250 mm,5 μm),with mobile phase consisting of water( A)-acetonitrile( B) at the flow rate of 1. 0 mL·min~(-1)( 0-10 min,0-1% B; 10-65 min,1%-3% B). The detection wavelength was 260 nm,the column temperature was controlled at 30 ℃,and the injection volume was 5 μL. The linear ranges of hypoxanthine,xanthine,uridine,inosine,guanosine and adenosine were 1. 025-20. 50( r = 0. 999 8),0. 545-10. 90( r = 0. 999 9),4. 051-81. 02( r = 0. 999 8),4. 044-80. 88( r= 0. 999 9),2. 075-41. 50( r= 0. 999 9),4. 032-80. 64( r = 0. 999 9) mg·L~(-1),respectively. The average recoveries of them( n = 6)were as follows: 102. 3%( RSD 2. 1%),101. 1%( RSD 2. 4%),97. 80%( RSD 1. 7%),101. 8%( RSD 1. 8%),98. 90%( RSD2. 0%) and 98. 10%( RSD 1. 4%),respectively. Each sample was processed by freeze-drying and sun-drying so as to compare the difference between the two drying methods. The contents of six index ingredients were significantly different between freeze-drying and sun-drying sample of C. sinensis. The total contents of six index ingredients in sun-drying sample were higher than that in the corresponding freeze-drying sample. This research results provide the scientific basis for the drying methods and quality evaluation of C. sinensis.


Subject(s)
Chromatography, High Pressure Liquid , Cordyceps , Chemistry , Desiccation , Freeze Drying , Nucleosides
9.
Acta Pharmaceutica Sinica ; (12): 598-603, 2018.
Article in Chinese | WPRIM | ID: wpr-779913

ABSTRACT

This study was designed to establish a method to obtain the fingerprint chromatogram for the quantitative determination of Cordyceps sinensis in different sizes, a comparison of Cordyceps sinensis from five places was made to analyze its similarity and the content of main nucleosides (uridine, inoside, guanosine and adenosine). The assay was performed on a Waters XSelect HSS T3 C18 (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of water (A)-acetonitrile (B) at the flow rate of 0.6 mL·min-1 (0-5 min, 0 B; 5-15 min, 0→10% B; 15-30 min, 10%→20% B; 30-33 min, 20%→50% B; 33-35 min, 50%→0 B; 35-40 min, 0 B). The detection wavelength was 260 nm and the column temperature was set at 30℃, and the injection volume was 5 μL. The results showed that there was no significant difference of the nucleosides in samples from the same place of the different sizes, but contents of the nucleosides variate a lot by production places. More data are required for further research. The method is proved for scientific and specific formulation of the standard in evaluation of circulated Cordyceps sinensis.

10.
Article in Chinese | WPRIM | ID: wpr-771670

ABSTRACT

This present study is to develop an HPLC method for simultaneous determination of four diester diterpenoid alkaloids, beiwutine, mesaconitine, hypaconitine and aconitine in the leaves of Aconitum kusnezoffii, so as to provide evidence of the quality control of this herb. The four constituents were measured on a Waters XBridge CC₁₈ column(4.6 mmχ250 mm, 5 μm). The mobile phase was acetonitrile-40 mmol·L⁻¹ ammonium acetate solution(adjusted pH to 10.5 with ammonia solution)(33:67) with isocratic elution at a flow rate of 1.0 mL·min⁻¹; the detection wavelength was 235 nm; the column temperature was 30 °C, and the injection volume was 10 μL. Next, this contents of the four diester diterpenoid alkaloids in 12 samples were 0.025 5-0.088 5, 0.039 1-0.071 5, 0.026 6-0.081 0 and 0.008 12-0.031 2 mg·g⁻¹, respectively. Next, this method has been successfully applied to the analysis of A. kusnezoffii folium in different harvest periods. The contents of the four alkaloids decreased primarily, and then increased with the postponing of harvest. The established method is proved to be accurate and sensitive for the determination of alkaloids in A. kusnezoffii folium, and may be useful for the quality improvement of this herbal medicine. Moreover, these results indicated the scientific significance for the toxicity and the suitable harvest time of this herb.


Subject(s)
Aconitine , Aconitum , Chemistry , Chromatography, High Pressure Liquid , Diterpene Alkaloids , Drugs, Chinese Herbal , Chemistry , Phytochemicals , Plant Leaves , Chemistry , Plants, Medicinal , Chemistry
11.
Article in Chinese | WPRIM | ID: wpr-690716

ABSTRACT

High price and difficult to get of reference substance have become obstacles to HPLC assay of ethnic medicine. A new method based on quantitative reference herb (QRH) was proposed. Specific chromatograms in fruits of Capsicum frutescens were employed to determine peak positions, and HPLC quantitative reference herb was prepared from fruits of C. frutescens. The content of capsaicin and dihydrocapsaicin in the quantitative control herb was determined by HPLC. Eleven batches of fruits of C. frutescens were analyzed with quantitative reference herb and reference substance respectively. The results showed no difference. The present method is feasible for quality control of ethnic medicines and quantitative reference herb is suitable to replace reference substances in assay.

12.
Article in Chinese | WPRIM | ID: wpr-690496

ABSTRACT

This study was performed to investigate the guaianolides from the aerial parts of Artemisia myriantha. The chemical constituents were isolated by chromatographic columns over silica gel, Sephadex LH-20, and ODS, as well as Semi-prep HPLC methods, and their structures were identified by NMR and MS data. Ten compounds were isolated and identified as follows: artemyriantholide E (1), tanaphillin (2), 1β, 10β-epoxydehydroleucodin (3), 5-hydroxyleucodin (4), dehydrocostuslactone (5), 3-O-methyl-iso-secotanapartholide (6), roxbughianin A (7), dehydroleucodin (8), arglabin (9), and 8α-acetoxyarglabin (10). Compound 1 was a new compound, and compounds 2-7 were isolated from this plant for the first time. Compound 3 exhibited selective cytotoxicity against human liver cancer (Bel-7402) with IC₅₀ value of 5.35 μmol·L⁻¹, and 6 against human gastric cancer (BGC-823) with IC₅₀ value of 2.68 μmol·L⁻¹, respectively.

13.
Article in Chinese | WPRIM | ID: wpr-687250

ABSTRACT

The present study is to develop an HPLC-ELSD method for simultaneous determination of three pairs of triterpenoid isomers, Ilexsaponin A₁, Ilexhainanoside D, Ilexgenin A, 3β, 19α-dihydroxyolean-12-ene-24, 28-dioic acid (ilexhainanin E) ursolic acid and oleanic acid in the leaf of Ilex hainanensis, which could provide evidence to the quality control of this herb. The six constituents were measured on a Waters XBridge C₁₈ column (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of methanol (A)- 0.5% formic acid in water (B) at a flow rate of 1.0 mL·min⁻¹ (0-18 min,70%-85% A,18-20 min,85%-95% A;20-35 min,95% A). The carrier gas was N₂, and the pressure was 2.8 L·min⁻¹. The drift tube in this experiment were set at 70 °C. The injection volume was 10 μL. The contents of the six triterpenoids in 6 samples were 3.7-8.5, 10.3 -22.1, 2.8-5.9, 7.8-14.1, 2.6-3.8 and 8.8-11.9 mg·g⁻¹, respectively. The established method is proved to be accurate and sensitive for the determination of triterpenoids in Ilicis Hainanensis Folium, and may be used for the quality improvement of this herb.

14.
Article in Chinese | WPRIM | ID: wpr-258483

ABSTRACT

This present study is to develop an HPLC method for simultaneous determination of eight hydroxyl naphthoquinones, shikonin, β-hydroxy-isovalerylshikonin, acetylshikonin, β-acetoxy-isovalerylshikonin, deoxyshikonin, isobutyrylshikonin, β,β'-dimethylacrylshikonin and isovalerylshikonin. The eight constituents were measured on a Waters Xbridge C18 column (4.6 mm×250 mm,5 μm) with isocratic elution of acetonitrile-0.05% formic acid solution (70∶30) at a flow rate of 1.0 mL•min⁻¹. The detection wavelength was 275 nm and the column temperature was 30 ℃. The results of content determination indicated that significant differences of the eight compounds exist in every part of Arnebia euchroma,in which the highest part was the root bark, followed with the root, then the stem residues. The content of the xylem of root and aerial part was lower than the above parts. The results provided scientific basis for the medicinal parts of A. euchroma.

15.
Article in Chinese | WPRIM | ID: wpr-335901

ABSTRACT

The present study is to compare specific chromatograms and main acitive components between wild and cultivated rhizomes of Paris polyphylla var. yunnanensis by HPLC. HPLC analysis was performed on a Waters XSelect HSS T3 C₁₈ clumn (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of acetonitrile (A)-water (B) at a flow rate of 1 mL•min⁻¹ (0-50 min,30%-50%A;50-80 min,50% A,80-85 min,50%-30%A;85-100 min,30% A). The detection wavelength was 203 nm and the column temperature was controlled at 30 ℃, and the injection volume was 10 μL. HPLC specific chromatograms of wild and cultivated rhizomes of P. polyphylla var. yunnanensis were established and nine steroidal saponins were simultaneously determined by the above method. The mean contents of paris saponin Ⅶ, paris saponin H and total average contents of four pennogenyl saponins in Rhizomes of wild samples were significantly higher than those of cultivated ones. However, this result is opposite from the average content of paris saponin Ⅰ and total average contents of five dioscins in the wild and cultivated samples. Because the significant differences occurred for the specific chromatograms and main active components between the wild and cultivated P. polyphylla var. yunnanensis, much more pharmacological and clinical researches are therefore necessary.

16.
Article in Chinese | WPRIM | ID: wpr-335757

ABSTRACT

This study is to establish the HPLC specific chromatogram and determine four main nucleosides of wild and cultivated Cordyceps sinensis. Uridine, inosine, guanosine and adenosine were selected as reference substance. HPLC analysis was performed on a Waters XSelect HSS T3 C₁₈ (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of water(A)-acetonitrile (B) at a flow rate of 0.6 mL•min⁻¹ (0-5 min,0% B;5-15 min,0%-10% B, 15-30 min,10%-20% B, 30-33 min, 20%-50% B, 33-35 min, 50%-0% B, 35-40 min, 0% B). The detection wavelength was 260 nm and the column temperature was controlled at 30 ℃, and the injection volume was 5 μL. HPLC specific chromatogram of wild and cultivated C. sinensis was established and four main nucleosides were simultaneously determined by the above method. Specific chromatograms and contents of four main nucleosides showed no significant differences between cultivated and wild C. sinensis. These results can provide scientific evidences for further development and utilization of cultivated C. sinensis.

17.
Article in Chinese | WPRIM | ID: wpr-275189

ABSTRACT

Twelve compounds were isolated from alcohol extracts of the rhizome of Homalomena occulta by using various chromatographic techniques including column chromatography onsilica gel and C₁₈ reverse-phase silica gel, and semi-preparative HPLC. Their structures were identified by physico-chemical properties and spectroscopic data analysis as 3α, 7α-dihydroxy-cadin-4-ene (1), 3-oxofabiaimbricatan (2), 3β, 4α-dihydroxy-7-epi-eudesm-11(13)-ene (3), integrifonol A(4), 1β, 6β-dihydroxy-7-epi-eudesm-11(13)-ene (5), 4β, 7β, 11-enantioeudesmantriol (6), epi-guaidiol (7), oplopanone(8), (-)-1β, 4β, 6α-trihydroxy-eudesmane (9),2α-hydroxyhomalomenol(10), (-)-T-muurolol (11) and hamalomenol A(12). Compounds 1-7 were obtained from the genus Homalomena for the first time and 11-12 were firstly reported from the species. Additionally, compounds 3, 5 and 8 displayed inhibitory effects against the lipopolysaccharide (LPS)-induced nitric oxide (NO) production in mouse macrophage RAW264.7 cells with IC₅₀ values of 6.51, 3.25, 7.78 μmol•L⁻¹, respectively.

18.
Article in Chinese | WPRIM | ID: wpr-258454

ABSTRACT

The present study is to investigate the chemical constituents from the aerial parts of Artemisia myriantha. The chemical constituents were isolated by column chromatographies over silica gel, Sephadex LH-20, ODS and Semi-prep HPLC, and the structures were identified by NMR and MS data. Thirteen known compounds were isolated and identified as: blumenol A (1),(+)-dehydrovomifoliol (2),(+)-3-hydroxy-β-ionone (3),(3R, 6R, 7E)-3-hydroxy-4, 7-megastigmadien-9-one (4),(-)-10-oxo-isodauc-3-en-15-oic acid (5),isoerivanin (6),eudesmafraglaucolide (7), artanomalide A (8),13-acetoxy-3β-hydroxy-germacra-1(10) E,4E,7(11)-trien-12,6α-olide (9),13-acetoxy-3β-tigloyl-germacra-1(10) E, 4E, 7(11)-trien-12, 6α-olide (10),13-acetoxy-3β-(3-methylbutanoyl)-germacra-1(10)E, 4E, 7(11)-trien-12, 6α-olide (11),3,9-diacetoxy-13-hydroxy-1(10), 4, 7(11)-germacratrien-12,6α-olide (12), and 8α-angeloyloxycostunolide (13). Compounds 1-6 and 13 were obtained from the genus Artemisia for the first time, and 7-9 and 12 were isolated from this plant for the first time. Compound 8 exhibited selective cytotoxicity against human colon cancer (HCT-8) and human gastric cancer (BGC-823) with IC₅₀ values of 2.33 and 4.53 μmol•L ⁻¹, respectively.

19.
Article in Chinese | WPRIM | ID: wpr-236097

ABSTRACT

This study is to establish the HPLC specific chromatogram and determine four main effective components of Lamiophlomis Herba and its counterfeit.Chlorogenic acid, forsythoside B, acteoside and luteoloside were reference substance.HPLC analysis was performed on a Waters XSelect C₁₈ column (4.6 mm×250 mm,5 μm).The mobile phase was acetonitrile-0.5% phosphoric acid solution (18∶82) with isocratic elution.The flow rate was 1.0 mL•min⁻¹, the detection wavelength was 332 nm and the column temperature was 30 ℃.Chemometrics software Chempattern was employed to analyze the research data.HPLC specific chromatogram of Lamiophlomis Herba from different samples were of high similarity, but the similarity of the HPLC specific chromatogram of its counterfeit were less than 0.65.Both of cluster and principal component analysis can distinguish certified products and adulterants.The HPLC specific chromatogram and contents of four effective components can be used for the quality control of Lamiophlomis Herba and its preparations.It provided scientific basis to standardize the use of the crude drug.

20.
Article in Chinese | WPRIM | ID: wpr-304887

ABSTRACT

In order to isolate and purify the reference compounds and improve the quality standard of ethnic medicine of Radix of Cynanchum otophyllum, the ethanol extracts were isolated by column chromatography onsilica gel, C₁₈ reverse-phase silica gel, and semi-preparative HPLC. Twelve compounds were isolated and their structures were elucidated as 2,4-dihydroxy-6-methoxyphenylethanone(1), 4,6-dihydroxy-2-methoxyphenylethanone(2), p-hydroxyacetophenone(3), baishouwubenzophenone(4), 2,4-dihydroxyacetophenone(5), 2,5-dihydroxyacetophenone(6), otophylloside A(7),otophylloside B(8), caudatin-3-O-β-D-cymaropyranosyl-(1→4)-β-D-digitoxopyranoside(9),caudatin-3-O-β-D-glucopyranosyl-(1→4)-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranosyl-(1→4)-β-D-digitoxopyranoside(10),qingyangshengenin-3-O-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranoside(11),caudatin-3-O-β-D-oleandropyranosyl-(1→4)-β-D-cymaropyranosyl-(1→4)-β-D-cymaropyranoside(12) on the basis of spectral analysis. Compounds 1 and 2 were isolated from the genus Cynanchum for the first time, and compounds 3-4, 9-12 were obtained from this plant for the first time.These compounds are main active components of Radix of C.otophyllum and can be used as reference substances for the quality control of this ethnic medicine.

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