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Study on separation of sulfonamides by capillary high-performance liquid chromatography and electrochromatography.

Rui-fen YANG ; Zhi-guo SHI ; Yu-qi FENG ; Shi-lu DA

Acta Pharmaceutica Sinica.2003;38(2):129-132.

AIMTo establish separation methods of five sulfonamides by using capillary high performance liquid chromatography(mu-HPLC) and electrochromatography. The effect of mobile phase varies such as methanol content, pH, buffer solution concentration and voltage on their chromatographic behavior and electroosmesis flow was investigated. Capillary electrochromatography (CEC) was compared with mu-HPLC at the same condition.

METHODSStationary phase was ODS, mobile phase was methanol and 2 mmol.L-1 H3PO4 buffer solution (pH 3.0-7.0), voltage was 0- -15 kV, flow rate was 10 microL.min-1, pressure was approximately 70 MPa and UV detection wavelength was 254 nm.

RESULTSSeparations on base line have been respectively accomplished for five sulfonamides by mu-HPLC with mobile phase of methanol-2 mmol.L-1 H3PO4 buffer solution (30:70) at pH 5.0 in 67 min, and CEC with the same mobile phase at -5 kV voltage in 25 min.

CONCLUSIONElectroosmesis flow of CEC decreased with the increase in methanol content, buffer solution concentration, increased with the increase in voltage and increase slightly with the increase in pH of mobile phase. Retention values (k) of solutes to be examined decreased with increasing methanol content of mobile phase in mu-HPLC and CEC. Retention values (k) of solutes increased slightly with increasing buffer solution concentration, decreased with increasing voltage in CEC. Trimethoprim(TMP) decreased obviously with increasing voltage in CEC. The effect of pH of mobile phase on retention values (k) was more complex. Five sulfonamides were separated at the same mobile phase condition by mu-HPLC and CEC. And separation speed of CEC was much faster than that of mu-HPLC. CEC was very fit for rapid separation of sulfonamides.

Anti-Infective Agents ; isolation & purification ; Buffers ; Chromatography, High Pressure Liquid ; methods ; Chromatography, Micellar Electrokinetic Capillary ; methods ; Hydrogen-Ion Concentration ; Sulfonamides ; isolation & purification ; Trimethoprim ; isolation & purification

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Determination of 9-nitrocamptothecin in rat plasma and tissues by high performance liquid chromatography.

Ke LI ; Da-fang ZHONG

Acta Pharmaceutica Sinica.2003;38(2):124-128.

AIMTo develop a sensitive, specific and accurate method for quantifying 9-nitrocamptothecin in rat plasma and tissues and to study the distribution of 9-nitrocamptothecin in rat tissues.

METHODSPlasma and tissue samples were prepared based on a simple liquid-liquid extraction and separation through a Hypersil BDS C18 column. The mobile phase for plasma samples and tissue samples consisted of a mixture of acetonitrile-water-formic acid (35:65:2) and a mixture of acetonitrile-water-formic acid (30:70:2), respectively. The UV detector was set at 370 nm.

RESULTSA linear calibration curve of 9-nitrocamptothecin in plasma was obtained in the concentration range of 25-1,600 micrograms.L-1, and the quantitation limit of plasma and tissues was 25 micrograms.L-1. A linear range of concentrations for 9-nitrocamptothecin in heart, lung, spleen, stomach, fat, womb, and ovary was 10-1,000 ng.g-1, and the quantitation limit was 10 ng.g-1. A linear range of concentrations for 9-nitrocamptothecin in brain, kidney, liver, intestine, smooth muscle, skeletal muscle, and tectical was 5-500 ng.g-1, and the quantitation limit was 5 ng.g-1. The intra- and inter-run precision was measured to be below 11%. The inter-run accuracy was less than 5% for the analyte. After i.v. administration of 9-nitrocamptothecin, the drug was distributed extensively in rat in vivo. The concentration in lung was the highest, and the drug was accumulated in lung and liver. Following ig administration, the concentration in stomach was higher than that in other organs.

CONCLUSIONThe method is shown to be accurate and convenient, and suitable for preclinical pharmacokinetic studies of 9-nitrocamptothecin.

Animals ; Antineoplastic Agents, Phytogenic ; blood ; pharmacokinetics ; Camptothecin ; analogs & derivatives ; blood ; pharmacokinetics ; Chromatography, High Pressure Liquid ; Female ; Liver ; metabolism ; Lung ; metabolism ; Male ; Rats ; Rats, Wistar ; Tissue Distribution

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Determination of adefovir in monkey plasma by liquid chromatography-tandem mass spectrometry.

Li-yan ZHAO ; Xiao-yan CHEN ; Yong ZHANG ; Han-yu YANG ; Da-fang ZHONG

Acta Pharmaceutica Sinica.2003;38(2):120-123.

AIMTo develop a sensitive and specific liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for the determination of adefovir in monkey plasma.

METHODSAdefovir and internal standard 9-(3-phosphonylmethoxypropyl) adenine were isolated from plasma by protein precipitation with methanol, then chromatographed by using a Diamonsil C18 column. The mobile phase consisted of methanol-water-formic acid (20:80:1). Electrospray ionization (ESI) source was applied and operated in the positive ion mode. Selected reaction monitoring (SRM) mode with the transitions of m/z 274-->m/z 162 and m/z 288-->m/z 176 were used to quantify adefovir and the internal standard, respectively.

RESULTSThe linear calibration curve was obtained in the concentration range of 0.02-4.00 mg.L-1. The lower limit of quantitation was 20 micrograms.L-1. The inter- and intra-day precision (RSD) was less than 5.8%, and the accuracy (relative error) was within +/- 4.5%. The method was successfully used in a pharmacokinetic study of adefovir dipivoxil in monkeys.

CONCLUSIONThe method is proved to be suitable for pre-clinical investigation of adefovir dipivoxil pharmacokinetics, which offers advantages of specificity and simple sample preparation compared with the previously reported methods.

Adenine ; analogs & derivatives ; blood ; pharmacokinetics ; Animals ; Antiviral Agents ; blood ; pharmacokinetics ; Biotransformation ; Chromatography, Liquid ; Macaca mulatta ; Organophosphonates ; Spectrometry, Mass, Electrospray Ionization

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Isolation and structural identification of phenylethanoid glycosides from Corallodiscus flabellata.

Xiao-ke ZHENG ; Jun LI ; Wei-sheng FENG ; Yue-feng BI ; Chun-ru JI

Acta Pharmaceutica Sinica.2003;38(2):116-119.

AIMTo study the chemical constituents from Corallodiscus flabellata.

METHODSThe compounds were isolated and purified by macroporous adsorption resin, silica gel column chromatography and identified on the basis of their physiochemical and spectral data.

RESULTSThree phenylethanoid glycosides (I-III) were obtained from the n-BuOH fraction of water-extracts. Their structures were elucidated as 3,4-dihydroxyphenylethanol-8-O-[beta-D-apiofuranosyl (1-->3)]-beta-D-glucopyranoside (I), 3,4-dihydroxyphenylethanol-8-O-[4-O-trans-caffeoyl-beta-D-apiofuranosyl (1-->3)-beta-D-glucopyranosyl-(1-->6)]-beta-D-glucopyranoside (II) and 3,4-dihydroxyphenylethanol-8-O-[beta-D-apiofuranosyl(1-->3)-beta- D-glucopyranosyl-(1-->6)]-beta-D-glucopyranoside (III).

CONCLUSIONCompounds I, II and III are new compounds.

Caffeic Acids ; chemistry ; isolation & purification ; Disaccharides ; chemistry ; isolation & purification ; Glycosides ; chemistry ; isolation & purification ; Magnoliopsida ; chemistry ; Molecular Structure ; Plants, Medicinal ; chemistry

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A new chromone glycoside from Cassia siamea lam.

Tai-sheng LÜ ; Yang-hua YI ; Hong-ying YUAN ; Zhi-guo ZHANG ; Wei LIU

Acta Pharmaceutica Sinica.2003;38(2):113-115.

AIMTo study the chemical constituents of the stem of Cassia siamea.

METHODSThe compounds were isolated by chromatography on silica gel, and identified on the basis of spectral analysis.

RESULTSFive compounds were isolated and identified as: beta-sitosterol (I), sucrose (II), n-octacosanol (III), 2-methyl-5-(2'-hydroxypropyl)-7-hydroxy-chromone-2'-O-beta-D-glucopyranoside (IV) and piceatannol (V).

CONCLUSIONCompound IV is a new compound. Compounds II, III and V were obtained from this plant for the first time.

Cassia ; chemistry ; Chromones ; chemistry ; isolation & purification ; Fatty Alcohols ; chemistry ; isolation & purification ; Monosaccharides ; chemistry ; isolation & purification ; Plant Stems ; chemistry ; Plants, Medicinal ; chemistry ; Stilbenes ; chemistry ; isolation & purification

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Prognosticating the region-selectivity in the O-methylation reaction of erythromycins by conformational search model.

Jin XU ; Ke-jiang LIN ; Qi-dong YOU

Acta Pharmaceutica Sinica.2003;38(2):108-112.

AIMIn order to find a way to prognosticate the region-selectivity in the O-methylation reaction of erythromycin and its derivatives, conformation search model of Hyperchem Pro 6.0 used in personal computer was used to establish it.

METHODSThe results of O-methylation reaction of compound 1, 2 and 3 showed the difference between 6-OH and 11-OH. Using the conformational search model of hyperchem, 1,000 conformations of compound 4, 5 and 6 were found with the parameter of dihedral angle. The 14-membered lactone ring was defined as a "plane". The position of carbonyl of 1- or 9- and hydroxyl of 6- or 11- is different, either "up-plane" or "down-plane". A statistic analysis of low-energy conformation clusters was used to sort these clusters by the parameter of the dihedral angle. The data is in accord with the results of the experiments.

RESULTSConformation numbers, energy minimum, energy average and position of the active groups of compounds 4, 5 and 6, the simplified structures of compound 1, 2 and 3, were given in Table 1. by sorting the dihedral angle.

CONCLUSIONThe interaction of the hydroxyl and carbonyl were analysed and found that O-methylation reactions of erythromycin and its derivatives were impacted by the space factor. The clusters of energy minimum, maximum number and "outside" were discussed. The selectivity of the O-methylation reaction of erythromycin and its derivatives can be prognosticated by analysing the parameter of the dihedral angle.

Automatic Data Processing ; Erythromycin ; chemistry ; metabolism ; Methylation ; Models, Molecular ; Molecular Conformation ; Molecular Structure

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Protective effect of puerarin on vascular endothelial cell apoptosis induced by chemical hypoxia in vitro.

Rui-li SHI ; Jian-jun ZHANG

Acta Pharmaceutica Sinica.2003;38(2):103-107.

AIMTo study the effect of puerarin on vascular endothelial cells apoptosis induced by chemical hypoxia-ischemia in vitro.

METHODSThe chemical hypoxia-ischemia model was performed by treating cultured bovine aortic endothelial cells (BAECs) with NaCN in glucose-free medium. Cell viability was determined by trypan blue staining. Cell apoptosis was defined by terminal deoxynucleotidyl transferase-mediated dUTP nick end labeling (TUNEL), flow cytometry and Hoechst 33342 staining. The expression of Caspase-3 in endothelial cells was detected by immunocytochemical method.

RESULTSChemical hypoxia-ischemia was shown to initiate bovine aortic endothelial cell apoptosis. Puerarin (0.5-3 mmol.L-1) was found to inhibit endothelial cell apoptosis effectively, and reduce the expression of Caspase-3 significantly.

CONCLUSIONPuerarin can protect apoptotic endothelial cells induced by chemical hypoxia-ischemia markedly and the effect was performed partly by decreasing Caspase-3 expression.

Animals ; Aorta, Thoracic ; cytology ; Apoptosis ; Caspase 3 ; Caspases ; metabolism ; Cattle ; Cell Hypoxia ; drug effects ; Cells, Cultured ; DNA Damage ; drug effects ; Endothelium, Vascular ; cytology ; drug effects ; Isoflavones ; pharmacology ; Protective Agents ; pharmacology

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Effect of ginkgolide B on platelet-activating factor induced activation of rat polymorphonuclear leukocytes.

Zhen-gui NIE ; Wen-jie WANG

Acta Pharmaceutica Sinica.2003;38(2):98-102.

AIMTo investigate the effect of ginkgolide B on PAF-induced adhesion, chemotaxis and degranulation of rat polymorphonuclear leukocytes (PMNs).

METHODSThe adhesion of rat PMNs to rat synovial cells (RSC) was measured with MTT colorimetry. The chemotaxis of PMNs was quantified with Boyden chamber method. The degranulation of rat PMNs was evaluated by determining the activity of released beta-glucuronidase.

RESULTSIn comparison with control, ginkgolide B at the concentration of 10 mumol.L-1 significantly inhibited the adhesion of PMNs to RSC by 71.74%. At the final concentration of 1-1,000 nmol.L-1, ginkgolide B dose-dependently inhibited the chemotaxis of PMNs stimulated with 10 nmol.L-1 platelet-activating factor (PAF), the IC50 was 4.84 nmol.L-1. At the final concentration of 0.01-10 mumol.L-1, ginkgolide B decreased the release of beta-glucuronidase in PMNs induced by 1 mumol.L-1 PAF in dose-dependent manner. The IC50 was 3.56 mumol.L-1.

CONCLUSIONGinkgolide B was found to significantly inhibit PAF-induced adhesion, chemotaxis and degranulation in rat polymorphonuclear leukocytes. These effects might be considered a part of the mechanisms underlying the antiinflammatory action of ginkgolide B.

Animals ; Anti-Inflammatory Agents, Non-Steroidal ; pharmacology ; Cell Adhesion ; drug effects ; Cells, Cultured ; Chemotaxis, Leukocyte ; drug effects ; Diterpenes ; isolation & purification ; pharmacology ; Drug Interactions ; Ginkgo biloba ; chemistry ; Ginkgolides ; Glucuronidase ; metabolism ; Lactones ; isolation & purification ; pharmacology ; Male ; Neutrophils ; drug effects ; physiology ; Plants, Medicinal ; chemistry ; Platelet Activating Factor ; antagonists & inhibitors ; pharmacology ; Rats ; Rats, Wistar

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Comparison of the effects of polysaccharides from wood-cultured and bag-cultured Ganoderma lucidum on murine spleen lymphocyte proliferation in vitro.

Li-zhen CAO ; Zhi-bin LIN

Acta Pharmaceutica Sinica.2003;38(2):92-97.

AIMTo compare the influences of wood-cultured Ganoderma lucidum polysaccharides (Gl-PS-WC) and bag-cultured Ganoderma lucidum polysaccharides (Gl-PS-BC) on the proliferation activities of murine spleen lymphocytes in vitro, and investigate whether Gl-PS-BC can be substituted for Gl-PS-WC.

METHODSMixed lymphocyte culture (MLC) reaction, lymphocyte proliferation induced by concanavalin A (Con A, 1 mg.L-1) or lipopolysaccharide (LPS, 5 mg.L-1), MLC reactions inhibited by immunosuppressive drugs, cyclosporine A (CsA, 0.1 mg.L-1), mitomycin (Mit C, 0.1 mg.L-1), or antitumor drug, etoposide (VP-16, 0.1 mg.L-1), were detected in the presence or absence of Gl-PS-WC and Gl-PS-BC in the concentration range of 0.2-12.8 mg.L-1.

RESULTSTwo kinds of polysaccharides were shown to promote MLC in the range of 0.2-12.8 mg.L-1, increase lymphocyte proliferation induced by Con A or LPS and antagonize the inhibitory effects of CsA, Mit C or VP-16 on MLC. No significant difference was observed between these two kinds of polysaccharides in selected concentrations.

CONCLUSIONGl-PS-WC and Gl-PS-BC showed similar effects on the proliferation activities of murine spleen lymphocytes in vitro.

Animals ; Cell Division ; drug effects ; Cell Separation ; Cyclosporine ; antagonists & inhibitors ; Lymphocyte Culture Test, Mixed ; Lymphocytes ; cytology ; drug effects ; Mice ; Mice, Inbred BALB C ; Mice, Inbred C57BL ; Plants, Medicinal ; chemistry ; growth & development ; Polysaccharides ; isolation & purification ; pharmacology ; Reishi ; chemistry ; growth & development ; Spleen ; cytology ; Wood

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A new vomiting animal model--mink.

Wang YUE ; Fang ZHANG ; Lei WANG ; Xuan FANG ; Yan-xia LIU ; Masaru MINAMI

Acta Pharmaceutica Sinica.2003;38(2):89-91.

AIMTo establish a new, reliable vomiting model in minks.

METHODSAdult male minks (Mustela vison) were randomly divided into groups (n = 6). Cisplatin, apomorphine, copper sulfate and X-radiation were used to establish vomiting model. Retching and vomiting were observed after the vomiting models were given anti-vomiting agents. After the behavioral experiment, assay of 5-HT in the ileum was performed by immunohistologic method.

RESULTSCisplatin 7.5 mg.kg-1 i.p., apomorphine 1.6 mg.kg-1 s.c. and copper sulfate 40 mg.kg-1 ig were shown to evoke vomiting. Retching and vomiting were significantly inhibited in ondansetron and metoclopramide pretreated minks (P < 0.05, P < 0.01).

CONCLUSIONAs a new vomiting model, minks may be of great value in studying vomiting mechanism and screening new antiemetic drugs.

Animals ; Antiemetics ; therapeutic use ; Apomorphine ; Cisplatin ; Copper Sulfate ; Disease Models, Animal ; Male ; Metoclopramide ; therapeutic use ; Mink ; Ondansetron ; therapeutic use ; Vomiting ; chemically induced ; drug therapy

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