Abstract：
:Rapamycin or sirolimus is a carboxylic lactone-lactam macrolide with a potent immunosuppressive activity. It can be successfully used to impregnate stents inserted in coronary arteries during surgical applications, preventing fatal infection and rejection adverse effect. The chemical stability of rapamycin in several organic-volatile solvents (acetone, chloroform, dichloromethane, hexane, ethyl alcohol, ethyl acetate, methyl alcohol, pentane and tetrahydrofurane) was established by HPLC-DAD-MS in reverse phase analysis. Results permitted to exclude rapamycin chemical degradation and to reveal a typical chemical isomerization, favoured in accordance to the solvent used. Two typical peaks appear, denominated beta and gamma, the time retention of which are, respectively, 11.3 and 15.0 min. Thanks to data recovered by NMR, spectrophotometric UV and mass analyses, it was possible to establish that both peaks correspond to two different isomeric forms of rapamycin. In addition, it was possible to establish that the relative percentage peak area varies according to the solvent and to the experimental time. The two isomeric forms are in equilibrium and each solvent concurs to differently displace this equilibrium versus one form rather than another, according to their both polarity index and aproticity.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Ricciutelli M,Di Martino P,Barboni L,Martelli Sdoi
10.1016/j.jpba.2006.02.009subject
Has Abstractpub_date
2006-06-07 00:00:00pages
1070-4issue
3eissn
0731-7085issn
1873-264Xpii
S0731-7085(06)00178-6journal_volume
41pub_type
杂志文章abstract：:The preparation method of metal based Indian traditional drugs involves conversion of a pure metal into its oxide by repeated high temperature calcination cycles. In this work, the effect of number of calcination cycles followed in the preparation of tin oxide based Ayurvedic drug, 'vanga bhasma' was studied by a syst...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.03.032
更新日期：2006-06-16 00:00:00
abstract：:The antigenic P64k protein from the pathogenic bacterium Neisseria meningitidis has been used as an immunological carrier in several conjugated vaccines. The aim of this report was to develop and validate a sensitive sandwich enzyme-linked immunosorbent assay (ELISA) for the quantification of recombinant p64k protein,...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.01.041
更新日期：2011-06-01 00:00:00
abstract：:3-(3-acetyl-4-hydroxyphenyl)-1,1-diethylurea (A-1354), is a synthetic intermediate of the beta-adrenergic blocker, celiprolol hydrochloride. A liquid chromatographic method has been developed and validated for the determination of bulk A-1354 and its potential impurities. High-low chromatography was used to improve th...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(91)80008-w
更新日期：1991-01-01 00:00:00
abstract：:A new sildenafil analog has been identified in the softgel shell of a dietary supplement. The compound was investigated by UV spectroscopy and high-resolution MS analysis, leading to the proposed structure 1-methyl-5-{5-[2-(4-methylpiperazin-1-yl)acetyl]-2-propoxyphenyl}-3-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.08.031
更新日期：2018-11-30 00:00:00
abstract：:A method for measuring a human immunodeficiency virus (HIV) cell membrane fusion inhibitor (T-20/Ro 29-9800) and its metabolite (M-20/Ro 50-6343) in human plasma by liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed. The relatively large peptide analytes and their corresponding deuterated (d(10)) ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2005.01.024
更新日期：2005-07-01 00:00:00
abstract：:Siberian ginseng (Eleutherococcus senticosus, Araliaceae) and roseroot (Rhodiola rosea, Rosaceae) are popular herbal supplements which have been shown to improve resilience to conditions such as stress and exhaustion. Using DNA barcoding methods we tested 25 Siberian ginseng and 14 roseroot products which are widely a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.11.025
更新日期：2018-02-05 00:00:00
abstract：:Huangqi Guizhi Wuwu Decoction (HGWWD), consisting of Radix Astragali, Cinnamomi Ramulus, Paeoniae Radix Alba, Zingiberis Rhizoma Recens and Jujubae Fructus, is a widely used Traditional Chinese Medicine (TCM) formula for the treatment of human blood impediment in China for nearly 2000 years. In order to make good and ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.03.022
更新日期：2019-06-05 00:00:00
abstract：:In this study, a green production method was used to obtain magnetic carbon nanodot/graphene oxide hybrid material (Fe3O4@C-nanodot@GO) for the magnetic solid phase extraction (MSPE) of ibuprofen (IBU) in human plasma prior to HPLC-DAD determination. For the first time in the literature, Fe3O4@C-nanodot@GO hybrid mate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.113001
更新日期：2020-02-05 00:00:00
abstract：:NMR spectra of urine from rats treated with a range of liver, kidney and testicular toxins at various doses were measured and classified using neural network methods. Toxin-induced changes in the levels of 18 low molecular weight endogenous urinary metabolites were assessed using a simple semi-quantitative scoring sys...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(95)01278-s
更新日期：1995-03-01 00:00:00
abstract：:Molecularly imprinted polymers (MIPs) for caffeic acid (CA) were prepared using 4-vinylpyridine and methacrylamide (MAM) as functional monomers, divinylbenzene as a crosslinker and acetonitrile-toluene (3:1, v/v) as a porogen by precipitation polymerization. The use of MAM as the co-monomer resulted in the formation o...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.12.052
更新日期：2016-08-05 00:00:00
abstract：:Concentrated solutions of doxycycline are often added to drinking water of animals for oral antibiotic therapy. However, stability concerns of doxycycline in solution involve an accurate selection of the solvent system to ensure that the active substance will remain within the acceptance range during the product shelf...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.06.054
更新日期：2018-09-10 00:00:00
abstract：:The topical administration of timolol as an ion-pair with octanoate was achieved by use of an oil-in-water microemulsion containing lecithin as a surfactant. The microemulsion, a solution of the ion-pair and a solution of timolol alone were instilled in the conjunctival sac of rabbits. A rapid method for the separatio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(89)80030-5
更新日期：1989-01-01 00:00:00
abstract：:Liquid chromatography (LC) and capillary electrophoresis (CE) methods were developed to perform the determination of residual sodium in mother liquors and successive washes of an active pharmaceutical ingredient (API). The addition of sodium chloride to the product solution results in rapid and complete crystallizatio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.07.020
更新日期：2007-07-27 00:00:00
abstract：:An automated on-line SPE and innovative fast polarity switch bioanalysis method employing dual-gradient liquid chromatography (DGLC) coupled with mass spectrometry (DGLC-MS/MS) was established and validated for the simultaneous determination of ferulic acid, ligustrazine and ligustilide in rat plasma after administrat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.08.038
更新日期：2014-01-01 00:00:00
abstract：:The 60 MHz (1)H NMR spectra of racemic 6,7-dichloro-5-methoxy-2-methyl-2-phenyl-1 indanone (1) have been studied with the achiral shift reagent, tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato) europium (III) (2) and the chiral reagents, tris[3-(trifluoromethylhydroxymethylene)-d-camphorato] europium (II...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(86)80065-6
更新日期：1986-01-01 00:00:00
abstract：:Monitoring amino acids and vitamins is important for understanding human health, food nutrition and the culture of mammalian cells used to produce therapeutic proteins in biotechnology. A method including ion pairing reversed-phase liquid chromatography with tandem mass spectrometry was developed and optimized to quan...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.08.036
更新日期：2016-01-05 00:00:00
abstract：:Indirect biomarkers of recombinant human growth hormone (rhGH), insulin-like growth factor-I (IGF-I), insulin-like growth factor-II (IGF-II), insulin-like growth factor binding proteins (IGFBP-2 and IGFBP-3) and insulin (C-peptide) were measured together with urinary parameters of renal damage (beta(2)-microglobulin a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.06.032
更新日期：2010-12-01 00:00:00
abstract：:Three methods are described for the simultaneous determination of mebeverine hydrochloride (MB) and sulpiride (SU) in combined pharmaceutical tablets. The first method depends on first-derivative ultraviolet spectrophotometry, with zero-crossing measurement method. The first derivative amplitudes at 214.2 and 221.6 nm...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00176-4
更新日期：1999-11-01 00:00:00
abstract：:A simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method was developed and validated for the quantification of olanzapine, atypical antipsychotic drug, in human plasma using loratadine as internal standard (IS). Following liquid-liquid extraction, the a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.01.040
更新日期：2006-06-07 00:00:00
abstract：:Several methods are reported for the simultaneous determination of diazepam and pyridoxine: two graphical methods (zero-crossing and derivative quotient spectra); and two numerical methods (multiple linear regression and partial least-squares regression). The methods have been applied in the concentration ranges 1.4-4...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(96)01844-4
更新日期：1996-11-01 00:00:00
abstract：:Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectro...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.03.005
更新日期：2018-05-30 00:00:00
abstract：:The binary phase diagram of (S)-(+)-4,4'-(1-methyl-1,2-ethandiyl)-bis-(2,6-piperazinedione), 1 (dexrazoxane), a cardioprotective agent, and of its (R)-(-)-enantiomer, 2, has been investigated by differential scanning calorimetry (DSC); the equimolecular mixture of 1 and 2 corresponds to a racemic compound (racemate) w...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(92)80007-a
更新日期：1992-01-01 00:00:00
abstract：:Pharmaceutical excipients containing volatile odor-active molecules can be used in pharmaceutical development to increase patients' compliance. However, capturing the molecular composition of these odor-active substances is challenging. Therefore, guidance for the analytical investigation of these excipients should be...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.01.033
更新日期：2015-06-10 00:00:00
abstract：:In this paper, binding interaction of 5-(ethoxycarbonyl)-6-methyl-4-(4-methoxyphenyl)-3,4-dihydropyrimidin-2(1H)-one (EMMD) with human serum albumin (HSA) under physiological conditions was investigated by using spectroscopy, isothermal titration calorimetry (ITC) and molecular modeling techniques. The results of spec...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.03.006
更新日期：2011-07-15 00:00:00
abstract：:The methyl- and ethylsulphoxide diastereoisomers (V and VI) of the corticosteroid tipredane (INN, I) have been shown to undergo further stereoselective S-oxidation to yield diastereoisomeric disulphoxides (II). Interactive computer optimisation software was employed to develop semi-preparative chromatography condition...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(96)01860-2
更新日期：1996-12-01 00:00:00
abstract：:Artesunate is the most widely used of the artemisinin derivatives. These drugs are being used increasingly throughout the tropical world, and are an essential component of the treatment of multi-drug resistant malaria. The recent and widespread appearance of counterfeit artesunate tablets in several countries in South...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(00)00360-5
更新日期：2000-12-01 00:00:00
abstract：:In this research, a facile and selective method was described to extract l-cysteine (l-Cys), an essential α-amino acid for anti-ageing playing an important role in human health, from human blood plasma sample. The importance of this research was the mild and time-consuming synthesis of zinc organic polymer (Zn-MOP) as...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.10.040
更新日期：2018-02-05 00:00:00
abstract：:A method for the determination of 4-aminophenol as an impurity in paracetamol (N-(4-hydroxyphenyl)-acetamide) by proton nuclear magnetic resonance ((1)H-NMR) spectroscopy has been developed. The (13)C-satellite from the protons in the ortho position from the hydroxyl group in paracetamol was used as an internal standa...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00086-9
更新日期：2002-07-01 00:00:00
abstract：:The extraction of diclofenac from spiked aqueous and plasma samples by liquid-liquid extraction (LLE) and solid phase extraction (SPE) methods is compared. The SPE methodology utilised a hydrophilic lipophilic balanced (HLB) copolymer as the extraction phase. Using a literature HPLC method, a calibration curve for dic...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00367-3
更新日期：2001-07-01 00:00:00
abstract：:A high-performance liquid chromatographic method for the determination of the theophylline solubilizer salicylamide-O-acetic acid has been developed in the range 0.5 to 10 microg/ml for human serum and 5 to 400 microg/ml for urine. Reversed-phase ion-pair chromatography was employed with tetrabutylammonium hydrogen su...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(85)80062-5
更新日期：1985-01-01 00:00:00
