Cinobufacino injection is a significant anti-tumor medicine for the treatment of various tumors in clinic, which was made from water extraction of the skin of Bufo bufo gargarizans. In present paper, HPLC-DAD-FT-ICR-MS method was used to identify the major bufadienolides in cinobufacino for the first time. Solid-phase extraction with dichloromethane and silica was used to enrich the total bufadienolides in cinobufacino. Based on the UV and high resolution MS/MS data, 33 bufadienolides were analyzed and characterized. Among them, eight compounds were identified by comparing with standard references unambiguously. This study elucidated the major bufadienolides in cinobufacino, which provided material foundation of cinobufacino and will be benefit for the further pharmacological research.
Amphibian Venoms ; chemistry ; Animals ; Bufanolides ; analysis ; chemistry ; Bufo bufo ; Chromatography, High Pressure Liquid ; Molecular Structure ; Spectrometry, Mass, Electrospray Ionization ; Tandem Mass Spectrometry

To obtain chemical constituent information of rat plasma after oral administration of Huang-Lian-Jie-Du Decoction (HLJDD), a LC-FT-ICR-MS method has been established, and both positive and negative ions scan modes were include in the analysis. By comparing their retention time, high resolution mass data of HLJDD extracts, blank plasma and dosed plasma, 38 constituents, including 22 prototype compounds and 16 metabolites, were detected in rat plasma after oral administration of HLJDD. In the 22 prototype compounds, 16 constituents were determined unambiguously by comparing with references. In the analysis of metabolites, phase II reactions like glucuronidation and sulfation were the major biotransformation pathways of HLJDD. M11 was observed as the only phase I metabolite in present experiment. The results will be beneficial for the further pharmacokinetics and pharmacological evaluations of HLJDD.
Administration, Oral ; Alkaloids ; blood ; Animals ; Biotransformation ; Chromatography, High Pressure Liquid ; Drug Combinations ; Drugs, Chinese Herbal ; administration & dosage ; isolation & purification ; metabolism ; Flavonoids ; blood ; Iridoids ; blood ; Male ; Plants, Medicinal ; chemistry ; Rats ; Rats, Sprague-Dawley ; Spectrometry, Mass, Electrospray Ionization ; Tandem Mass Spectrometry

Objective To investigate and evaluate the changes of T lymphocytes and red cell immunity of peripheral blood in patients with primary hepatocyte carcinoma (PHCC) after radiofrequency ablation(RFA) treatment. Methods The pre- and post- RFA(3d,7d,14d) peripheral blood T lymphocyte subsets(T3,T4,T8,T4/T8) and red cell immunity (RBC C3 receptor flower and RBC-immuocomplex formation rate) were investigated in 120 patients with PHCC treated by RFA. Results On 7d, 14d after RFA, T3, T4 lymphocytes and T4/T8 were higher than those on preoperative day significantly(P

Autophagy is a common phenomenon which widely ex-ists in eukaryotic cells. Researches have shown that autophagy plays a critical role in maintaining cellular hemostasis, cell com-ponents update and keeping a normal physiological state. In re-cent years, the study has found that autophagy is closely related to the growth, the development of cardiovascular diseases and tumors. Further studies show that in different pathological condi-tions, autophagy could both promote angiogenesis and inhibit the formation of blood vessels. Therefore, it is particularly critical to elucidate the mechanisms of autophagy in the regulation of angio-genesis in different pathological conditions. The role of autophagy in cardiovascular diseases especially in the regulation of angio-genesis is discussed in this paper. Besides, the paper also in-cludes the discussion about the mechanisms of autophagy in the regulation angiogenesis, which may provide references for follow-up research and clinical treatment.

OBJECTIVETo compare the solubilities of ephedrine and d-pseudo-ephdrine in the compound of traditional Chinese drugs--Maxing Shigan decoction with and without ultramicro-pulverizations using a RP-HPLC procedure.

METHODThe analytical column was a YMC ODS-C18(4.6 mm x 150 mm,4 microm). A mixture of water-acetonitrile-sodium dodecyl sulfate-phosphorous acid (650:350:5:1) was used as the mobile phase at flow rate of 1.5 mL x min(-1). The column temperature was 50 degrees C and the wavelength was 210 nm.

RESULTIn this way, ephedrine and d-pseudo-ephedrine of the compound samples can be separated well and showed significant differences before and after the ultramicro-pulverizations.

CONCLUSIONFor the Maxing Shigan decoction, the dissolution rates and solubilites of ephedrine and d-pseudo-ephedrine ultramicro-pulverization were greatly improved.

Calcium Sulfate ; chemistry ; Drug Combinations ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; Ephedra ; chemistry ; Ephedrine ; analysis ; chemistry ; Glycyrrhiza uralensis ; chemistry ; Particle Size ; Plants, Medicinal ; chemistry ; Powders ; Prunus ; chemistry ; Solubility ; Technology, Pharmaceutical ; methods

Cinobufacino injection is purified from water extraction of the skin of Bufo bufo gargarizans, which has been widely used for various cancers in clinic with significant anti-tumor effects. Bufadienolides were regarded as the main active constituents of cinobufacino injection in previous reports. In present study, 6 bufadienolides were isolated and purified from Cinobufacino injection. Their structures were identified as 3-epi-ψ-bufarenogin (1), ψ-bufarenogin (2), 3-epi-arenobufagin (3), arenobufagin (4), 3-epi-gamabufotalin (5), and 3-oxo-arenobufagin (6), separately. Among them, 1 and 3 were new compounds, 5 and 6 were new natural products. Compounds 1, 2 and compounds 3, 4 were two pairs configuration isomers at C-3, separately.
Animals ; Bufanolides ; chemistry ; isolation & purification ; Bufo bufo ; Injections ; Skin ; chemistry

In order to clarify the metabolism pathways of scandoside methyl ester, the analysis of metabolites profiling in four kinds of liver microsomes was performed by using an ultra-performance liquid chromatography/ electrospray-tandem mass spectrometry (UPLC-ESI-MS). The data obtained from the 0 h-incubation and the 2 h-incubation were compared and analyzed. After incubation, 5 metabolites of scandoside methyl ester were found in rat, Beagles, rhesus monkey and human liver microsome. The results showed that scandoside methyl ester's major metabolic pathway in the liver microsomes is hydrolysis, oxidation and reduction reactions, and there are certain kinds differences between species. The study provides a research base for further research about iridoid compounds in vivo metabolic pathways.
Animals ; Chromatography, High Pressure Liquid ; Dogs ; Esters ; metabolism ; Humans ; Iridoids ; metabolism ; Macaca mulatta ; Microsomes, Liver ; metabolism ; Rats ; Spectrometry, Mass, Electrospray Ionization

OBJECTIVETo determine the optimum technical parameters through controlling the different factors and the content of Dripping Pill.

METHODTime of dissolution, spherical degree and pill weight as parameters, the influential factors were investigated by orthogonal test and then to determine the content of liensinine, isoliensinine, neferine in plumula nelumbinis Alkaloid Dripping Pill.

RESULTThe optimum condition: 75% PEG4000 as matrix, methyl-silicon oil as refrigerant, 4 cm dripping distance, 10 degrees C refrigerant, 30 drippings per minute.

CONCLUSIONThe good quality pills can be produced through this process and the HPLC determination method is simple, reliable and can be used in the quality control of plumula nelumbinis Alkaloid Dripping Pill.

Alkaloids ; analysis ; chemistry ; Benzylisoquinolines ; analysis ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Isoquinolines ; analysis ; chemistry ; Microspheres ; Nelumbo ; chemistry ; Particle Size ; Phenols ; analysis ; chemistry ; Plants, Medicinal ; chemistry ; Polyethylene Glycols ; chemistry ; Quality Control ; Seeds ; chemistry ; Solubility ; Technology, Pharmaceutical ; methods

OBJECTIVETo optimize the molding formula of refined Xiong-gui sustained release pills, types and assorted dosages of water-soluble and non water-soluble drug carrier were studied.

METHODAn orthogonal design was performed to sift the pill formulation. The processing conditions were determining in terms of roundness, hardness, viscosity, fluidity, easily drop.

RESULT AND CONCLUSIONAccording to the final optimal formula, the amount of drug release can be detected instantly, while remaining over 80% at 10 h.

4-Butyrolactone ; analogs & derivatives ; analysis ; Angelica sinensis ; chemistry ; Delayed-Action Preparations ; Drug Combinations ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; Ligusticum ; chemistry ; Plants, Medicinal ; chemistry ; Technology, Pharmaceutical ; methods

OBJECTIVETo isolate and identify the chemical constitutents in roots of Jasminum sambac.

METHODThe compounds were isolated by means of chromatography and the structures were identified on the basis of physical and spectral data.

RESULTDotriacontanoic acid, dotriacontanol, oleanolic acid, daucosterol and hesperidin were elucidated.

CONCLUSIONAll compounds were found in this plant for the first time.

Hesperidin ; chemistry ; isolation & purification ; Jasminum ; chemistry ; Oleanolic Acid ; chemistry ; isolation & purification ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Sitosterols ; chemistry ; isolation & purification