1.Studies on quality standard of PsL 5F injections.
Ying-Nian LV ; G G CHEN ; Xian-Ling GONG ; Ke-Feng WU ; Nian-Ci LIANG
China Journal of Chinese Materia Medica 2008;33(20):2343-2346
OBJECTIVETo establish the quality standard of PsL injections containing mainly 5F (ent-11alpha-hydroxy-15-oxo-kaur-16-en-19-oic-acid).
METHODThe identification of PsL was performed by thin-layer chromatography, and the content was determined by HPLC. The column was Hypersil C18 (4.6 mm x 250 mm, 5 microm), the mobile phase was the mixture of methane-water-acitic acid (55:45: 0.045) with a flow rate of 1.0 mL x min(-1), the detective wavelength was 254 nm, and the column temperature was maintained at 35 degrees C. The pH value and K+ content of the three batchs injection were determined with pH meter and flame photometric meter, and the contents of tannin, protein, oxalic acid salt and heavy metals were detected by deferent methods.
RESULTThe TLC method was suitable for the identification of PsL5F. The linearity for 5F was obtained over the range of 30-240 microg x mL(-1) (r = 0.999 8), the average recovery of 5F was 99.8%. The injections were of pH value range from 7.80 to 8.20, K+ contents less than 10 mmol x L(-1), and the contents of tannin, protein, oxalic acid salt and heavy metals were qualified with the Chinese pharmacopoeia, respectively.
CONCLUSIONIt's sensitive and reliable that can be used as quality control methods of PsL5F injections.
Chromatography, High Pressure Liquid ; Chromatography, Thin Layer ; Diterpenes ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Injections ; Reproducibility of Results
2.Analysis of the diterpenoids in the extract of Pteris semipinnata L by HPLC-APCI-MS.
Yi-feng DENG ; Nian-ci LIANG ; Tong LIANG
Acta Pharmaceutica Sinica 2002;37(6):444-446
AIMTo establish an accurate and reliable method for quantitative analysis of the diterpenoids in Pteris semipinnata L.
METHODSA quadruple mass spectrometer coupled with atmospheric pressure chemical ionization interface was employed as a detector for HPLC. As to MS detector, selective ion monitoring (SIM) scan mode was used. For ent-11 alpha-hydroxy-15-oxo-kaur-16-en-19-olic acid (5F) and ent-11 alpha-hydroxy-15-oxo-kaur-16(R) methyl-19-olic acid (4F), the majority of the diterpenoids in Pteris semipinnata L, the [M-H]-1 ion were observed, and the [M-H2O-H]-1 ion could be observed from the collision-induced dissociation spectua. [M-H]-1 was selected as the SIM ion in quantification, the mobile phase and the MS conditions were optimized. The mobile phase of HPLC was 30% CH3CN-70% 2 mmol.L-1 NH4Ac, analytical column was Diamonsil ODS (4.6 mm x 150 mm), flow rate 1.0 mL.min-1, inject volume 5 microL. The area of ion flow peak were used for quantitative determination. As an example of its application, this method was used to determine the content of 5F as an antitumor diterpenoid in Pteris semipinnata L.
RESULTSThe content of 5F accounted 1.18 mg.g-1 in Pteris semipinnata L sample. For 5F, RT is about 4.3 min, the standard curve showed good linearity over the range of 0.05-2.5 micrograms, gamma = 0.9998 (n = 5); the recovery was 97.8% (n = 5); the limit of detection was 0.4 ng (inject 5 microL).
CONCLUSIONThis method is highly sensitive, accurate and fast, which can be applied to study the antitumor drug of diterpenoids in Pteris semipinnata L and to establish the raw herb standard.
Antineoplastic Agents, Phytogenic ; analysis ; chemistry ; pharmacology ; Chromatography, High Pressure Liquid ; methods ; Diterpenes ; analysis ; chemistry ; pharmacology ; Gas Chromatography-Mass Spectrometry ; Molecular Structure ; Plants, Medicinal ; chemistry ; Pteris ; chemistry ; Quality Control
3.Inhibitory effect and kinetic analysis of sodium quercetin-7,4'-disulphate on recombinant human protein kinase CK2 holoenzyme.
Xin-guang LIU ; Nian-ci LIANG ; Wen LIU ; Ji SHE ; Li-er MO
Acta Pharmaceutica Sinica 2002;37(3):165-168
AIMTo study the direct effect and kinetics of sodium quercetin-7,4'-disulphate (SQDS) on recombinant human protein kinase CK2 holoenzyme.
METHODSThe recombinant human CK2 holoenzyme activity was assayed by detecting incorporation of 32P of [gamma-32P] ATP into the substrate in various conditions.
RESULTSThe recombinant human CK2 was a second messenger (Ca2+, cAMP and cGMP) independent protein kinase. The characterization and function of the reconstituted holoenzyme were consistent with those of native CK2. SQDS was shown to strongly inhibit the holoenzyme activity of recombinant human protein kinase CK2 with an IC50 of 4.4 mumol.L-1, which was more effective than DRB and A3, known CK2 special inhibitors. Kinetic studies of SQDS on recombinant human CK2 showed: the inhibition was competitive with ATP and noncompetitive with casein.
CONCLUSIONSQDS is a potent inhibitor of protein kinase CK2. This study provide experimental basis for the development of more effective inhibitors of CK2 and for clinical application of SQDS in the future.
Casein Kinase II ; Dichlororibofuranosylbenzimidazole ; pharmacology ; Enzyme Inhibitors ; pharmacology ; Humans ; Kinetics ; Protein-Serine-Threonine Kinases ; antagonists & inhibitors ; metabolism ; Quercetin ; analogs & derivatives ; pharmacology ; Recombinant Proteins ; antagonists & inhibitors ; metabolism
4.Advances in study on chemical constituents and pharmacological activities of plants of genus Pteris.
Xian-Ling GONG ; Zhi-Hong CHEN ; Nian-Ci LIANG
China Journal of Chinese Materia Medica 2007;32(14):1382-1387
The main chemical constituents in plants of genus pteris include diterpenoids, diterpenoid glycosides, flavonoids, flavonoid glycosides, sesquiterpenoids and volatile oils, etc. Some of extracts show the following activities, such as antitumor, antifungi and antibacteria. Some of compounds have inhibitory effect on platelet aggregation and antiinflamatory action. The latest progress on chemical constituents and pharmacological activity were reviewed in the paper. Main problems and study directions in future of pteris were indicated.
Animals
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Anti-Bacterial Agents
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isolation & purification
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pharmacology
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Antifungal Agents
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isolation & purification
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pharmacology
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Antineoplastic Agents, Phytogenic
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isolation & purification
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pharmacology
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Diterpenes
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chemistry
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isolation & purification
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Drugs, Chinese Herbal
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chemistry
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isolation & purification
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pharmacology
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Flavonoids
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chemistry
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isolation & purification
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Humans
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Molecular Structure
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Plants, Medicinal
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chemistry
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Pteris
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chemistry
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Sesquiterpenes
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chemistry
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isolation & purification