Abstract：
:A rapid tandem mass spectrometric (MS-MS) method for the quantification of Oxcarbazepine (OXB) in human plasma using imipramine as an internal standard (IS) has been developed and validated. Chromatographic separation was achieved isocratically on a C18 reversed-phase column within 3.0 min, using a mobile phase of acetonitrile-10 mM ammonium formate (90 : 10 v/v) at a flow rate of 0.3 ml/min. Quantitation was achieved using multiple reaction monitoring (MRM) scan at MRM transitions m/z 253>208 and m/z 281>86 for OXB and the IS respectively. Calibration curves were linear over the concentration range of 0.2-16 mug/ml (r>0.999) with a limit of quantification of 0.2 mug/ml. Analytical recoveries of OXB from spiked human plasma were in the range of 74.9 to 76.3%. Plackett-Burman design was applied for screening of chromatographic and mass spectrometric factors; factorial design was applied for optimization of essential factors for the robustness study. A linear model was postulated and a 2(3) full factorial design was employed to estimate the model coefficients for intermediate precision. More specifically, experimental design helps the researcher to verify if changes in factor values produce a statistically significant variation of the observed response. The strategy is most effective if statistical design is used in most or all stages of the screening and optimizing process for future method validation of pharmacokinetic and bioequivalence studies.
journal_name
Chem Pharm Bull (Tokyo)journal_title
Chemical & pharmaceutical bulletinauthors
Srinubabu G,Ratnam BV,Rao AA,Rao MNdoi
10.1248/cpb.56.28subject
Has Abstractpub_date
2008-01-01 00:00:00pages
28-33issue
1eissn
0009-2363issn
1347-5223pii
JST.JSTAGE/cpb/56.28journal_volume
56pub_type
杂志文章abstract：:This report describes the synthesis and antiviral effects of (6'R)-6'-C-ethynyl, -ethenyl, and -ethyl derivatives of neplanocin A (7a, 8a, and 9a, respectively) and the corresponding 6'S-diastereomers (7b, 8b, and 9b, respectively), as examples of 6'-C-substituted analogues of neplanocin A. Grignard reaction of the 6'...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.45.1163
更新日期：1997-07-01 00:00:00
abstract：:Two sensitive and selective spectrofluorimetric and spectrophotometric stability-indicating methods have been developed for the determination of some non-steroidal anti-inflammatory oxicam derivatives namely lornoxicam (Lx), tenoxicam (Tx) and meloxicam (Mx) after their complete alkaline hydrolysis. The methods are ba...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.54.653
更新日期：2006-05-01 00:00:00
abstract：:A series of novel 1-(6,7-dimethoxy-4-quinazolinyl)piperidines carrying substituted hydantoin and 2-thiohydantoin rings was synthesized and examined for cardiotonic activity in anesthetized dogs. Introduction of isopropyl and sec-butyl group at the 5-position of the hydantoin and thiohydantoin rings led to potent inotr...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.38.3014
更新日期：1990-11-01 00:00:00
abstract：:Anti-tauro 1 beta-hydroxycholic acid antisera were prepared by immunizing rabbits with N-(1 beta,3 alpha, 7 alpha, 12 alpha-tetrahydroxy-5 beta-cholan-24-oyl)-2- aminopropionic acid-bovine serum albumin (BSA) conjugate. The antisera raised had high affinity (1.25-1.46 x 10(9) M-1) and specificity for conjugated 1 beta...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.40.1835
更新日期：1992-07-01 00:00:00
abstract：:A series of about fifty novel 5-arylfuro[2,3-d]pyrimidine derivatives were synthesized as potential inhibitors of dihydrofolate reductase (DHFR) arising from different species. Weak enzyme inhibition was observed for most of the compounds, with only a few reaching IC50 values less than 30 microM. With regards to antib...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.47.156
更新日期：1999-02-01 00:00:00
abstract：:Chemical examination of a Chinese soft coral Lobophytum pauciflorum resulted in the isolation of seven new biscembranoids, named lobophytones H-N (1-7). Their structures were determined by interpretation of 1D- and 2D-NMR (correlation spectroscopy (COSY), heteronuclear single quantum coherence (HSQC), heteronuclear mu...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.58.1591
更新日期：2010-12-01 00:00:00
abstract：:The objective of present work was to enhance the solubility and bioavailability of poorly aqueous soluble drug Irbesartan (IBS). The solid dispersions were prepared by spray drying method using low viscosity grade HPMC E5LV. Prepared solid dispersions were characterized by dissolution study, fourier transform infrared...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.59.438
更新日期：2011-01-01 00:00:00
abstract：:Two new diarylheptanoids, designated muricarpones A and B, together with three known diarylheptanoids, 1,7-di-(3',4'-dihydroxyphenyl)-4-hepten-3-one, 1-(3',4'-dihydroxyphenyl)-7-(4''-hydroxyphenyl)-4-hepten-3-one, and 1,7-bis(p-hydroxyphenyl)-4-hepten-3-one, were isolated from the rhizomes of Amomum muricarpum ELMER (...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.54.139
更新日期：2006-01-01 00:00:00
abstract：:1,4-Oxazepine formation reactions of 1,8-naphthyridine derivatives (1-4) with peroxy acid have been studied using a semiempirical MO method (AM1) and an ab initio molecular orbital method (Gaussian 94). The energies of molecules involved in the reaction paths were calculated and the transition states related to experi...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.48.755
更新日期：2000-05-01 00:00:00
abstract：:Targeted protein degradation by small molecules is an emerging modality with significant potential for drug discovery. We previously developed chimeric molecules, termed specific and non-genetic inhibitor of apoptosis protein (IAP)-dependent protein erasers (SNIPERs), which induce the ubiquitylation and proteasomal de...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.c18-00567
更新日期：2019-03-01 00:00:00
abstract：:A series of 5-(4-aryl- or 4-arylcarbonylpiperazin-1-yl)-5-deoxy-1,4: 3,6-dianhydro-L-iditol 2-nitrates was prepared in order to obtain orally active, nitrate-type vasodilators with reduced side effects. Our drug design was based on a small reduction in the lipophilicity compared to that of 5-deoxy-5-[4-(3-phenylthiopr...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.41.1100
更新日期：1993-06-01 00:00:00
abstract：:Hot aqueous extracts of 134 Chinese crude drugs were subjected to screening for inhibitory activity on K+ contracture of guinea pig taenia coli, and significant activity was observed in 17 crude drugs. Chemical investigations of two crude drugs, Kakko and Ubai, which originate from Pogostemon cablin and Prunus mume, r...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.37.345
更新日期：1989-02-01 00:00:00
abstract：:Enzymatic functions are often altered during disease onset and progression, and therefore chemical-biological studies, which utilize chemical knowledge to discover novel protein functions, are often employed to find proteins with functions closely related to disease phenotypes. Such studies are known as forward chemic...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章,评审
doi：10.1248/cpb.c17-00144
更新日期：2017-01-01 00:00:00
abstract：:We have identified a novel cardiac steroid, 11,19-epoxy-19-methoxytelocinobufagin, named marinosin (1), in the skin of the toad, Bufo marinus (L.) Schneider. The treatment of compound 1 with 50% CH3CN containing 0.1% trifluoroacetic acid yielded a 11 alpha-hydroxyhellebrigenin (2), which has not previously been isolat...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.45.249
更新日期：1997-02-01 00:00:00
abstract：:A method for the preparation of insulin derivatives having protected sulfhydryl group(s) on definite site(s) on the molecule which uses anion-exchange high performance liquid chromatography on a TSKgel DEAE-2SW column for separation is described. Porcine insulin reacts with N-succinimidyl S-acetylthioacetate to afford...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.40.957
更新日期：1992-04-01 00:00:00
abstract：:We previously reported an increase in aminobutyrate aminotransferase (GABA-T) activity in the cerebrum of Alzheimer patients. In the present study, we investigated whether such findings are common in the usual aging process as well. We examined the activity of various enzymes, which were examined in the previous study...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.38.1750
更新日期：1990-06-01 00:00:00
abstract：:Five glycyrrhetinic acid (Ib) derivatives have been synthesized to try to improve the antioxidant activity. Their in vitro antioxidant activities were studied using a cytochrome P450/NADPH reductase system from rat liver microsomes. The generation of microsomal free radicals was followed by oxidation of the DCFH-DA pr...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.52.1436
更新日期：2004-12-01 00:00:00
abstract：:Phytochemical investigation of the leaves of Umbilicus pendulinus afforded in addition to 2-O-caffeoyl malate, isoquercitrin and Z-venusol, the new isomer E-venusol. Special NMR experiments were carried out to elucidate the configuration of the two latter compounds. ...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.48.1768
更新日期：2000-11-01 00:00:00
abstract：:Four new prenylated bibenzyls, named aglaiabbrevins A-D (2, 4-6), were isolated from the leaves of Aglaia abbreviata, along with two known related analogues, 3,5-dihydroxy-2-[3,7-dimethyl-2(E),6-octadienyl]bibenzyl (7) and 3,5-dihydroxy-2-(3-methyl-2-butenyl)bibenzyl (8). The structures of the new compounds were eluci...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.c16-00868
更新日期：2017-01-01 00:00:00
abstract：:All-methylated isorugosin B was synthesized via two-step esterification between optically active valoneic acid and glucose derivatives. ...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.58.435
更新日期：2010-03-01 00:00:00
abstract：:In this study, the interactions of different groups substituted isoeuxanthone derivatives with calf thymus DNA (ct DNA) were investigated by spectrophotometric methods and viscosity measurements. Results indicated that the xanthone derivatives could intercalate into the DNA base pairs by the plane of xanthone ring and...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.c13-00789
更新日期：2014-01-01 00:00:00
abstract：:This paper describes syntheses and doxorubicin-inclusion abilities of beta-cyclodextrin (CyD) derivatives with a hydroquinone alpha-glycoside residue attached at the primary side. The hydroquinone glycoside having an alpha-D-glucosidic or 2-acetamido-2-deoxy-alpha-D-glucosidic linkage became a useful component for pro...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.57.74
更新日期：2009-01-01 00:00:00
abstract：:A HPLC method for the simultaneous determination of 11 triterpene saponins with four-type aglycones (protopanaxadiol, protopanaxatriol, ocotillol and oleanolic acid types) in Ginseng drugs was developed and validated. Using a gradient of acetonitrile and 10 mM K-phosphate buffer (pH 5.80) as the mobile phase and UV de...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.52.995
更新日期：2004-08-01 00:00:00
abstract：:Antimutagenic activity-guided fractionation of an extract prepared from the thorns of Gleditsia sinensis LAM. led to the isolation of one triterpenoid and four steroids, which were identified as D:C-friedours-7-en-3-one (1), stigmast-4-ene-3,6-dione (2), stigmastane-3,6-dione (3), stigmasterol (4), and beta-sitosterol...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.53.561
更新日期：2005-05-01 00:00:00
abstract：:Two new phenolic amides, pharnilatins A (1) and B (2), were isolated from the seeds of Pharbitis nil. These new compounds possess a p-coumaroyl unit with a structurally unique side chain, (2S,3S)-2,3-dihydroxyputrescine. The chemical structures and absolute stereochemistries of the new compounds were determined on the...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.58.1532
更新日期：2010-11-01 00:00:00
abstract：:New gamma-pyrones, 9'-oxopodopyrone (3) and 8-methyl-9'-oxopodopyrone (4) were isolated from the leaves of Gonystylus keithii, along with known gamma-pyrones, 10'-oxopodopyrone (1) and 8-methyl-10'-oxopodopyrone (2). These gamma-pyrones markedly inhibited the bovine parathyroid hormone (PTH)-induced Ca release from ne...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.45.1046
更新日期：1997-06-01 00:00:00
abstract：:A series of phthalazine and 1,2,3-benzotriazine derivatives which have heterocyclylpiperidino groups was synthesized and tested for cardiotonic activity in anesthetized dogs. Several 6,7-dimethoxyphthalazine derivatives showed relatively potent cardiotonic activity comparable to that of amrinone. ...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.38.2179
更新日期：1990-08-01 00:00:00
abstract：:A new route to (+)-estrone has been developed starting from the chiral building block having a bicyclo[3.2.1]octane framework based on the inherent stereochemical chemical nature of the chiral building block. ...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.51.104
更新日期：2003-01-01 00:00:00
abstract：:Four new cycloart-7-ene triterpenol arabinosides, bugbanosides C-F, were isolated from the underground parts of Cimicifuga simplex Wormsk. (Ranunculaceae). The structures were elucidated as 12beta-acetoxy-3beta,15alpha,-24R,25-tetrahydroxy-16,23-dione-cycloart-7-ene 3-O-alpha-arabinopyranoside, 12beta-acetoxy-24R,25-e...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.49.437
更新日期：2001-04-01 00:00:00
abstract：:Two sesterterpenes, deoxymanoalide (1) and deoxysecomanoalide (2), were isolated from the nudibranch Chromodoris willani collected in Okinawa and their structures determined on the basis of spectroscopic data and chemical conversions. The mollusk feeds on a sponge containing manoalide (3) and secomanoalide (4) and is ...
journal_title：Chemical & pharmaceutical bulletin
pub_type： 杂志文章
doi：10.1248/cpb.57.885
更新日期：2009-08-01 00:00:00
