Abstract：
:Gamma-hydroxybutyric acid (GHB) and its "pro-drugs", gamma-butyrolactone (GBL) and 1,4 butanediol (1,4-BD), are drugs of abuse with depressant effects on the central nervous system. Many analytical methods have been proposed for the quantitative determination of these compounds mainly in biological matrices but only few have been addressed to dietary supplements and foods. Facile synthesis of the GBL and 1,4-BD isotopologues are available by "one pot" Ru-catalyzed homogeneous deuteration of dicarboxylic acids. In this work we propose a new method for determination of GHB, GBL and 1,4-BD in commercially available dietary supplements, based on isotope dilution mass spectrometry (ID-MS). The procedure involves a simple extraction of sample with acidic acetonitrile and direct analysis by GC-ID-MS method without any purification or derivatization. Indeed, the proposed method takes advantage of the complete conversion of GHB (free acid or its salts) to GBL, allowing the quantification of GHB and its pro-drugs. Five levels for each calibration curve have been prepared by diluting working solutions of the analytes to obtain concentrations ranging from 1 to 20mg/mL. The validation procedures have shown an accuracy between 88% and 99% and a precision between 7.3% and 2.9% of each analyte in the sample matrix. Positive ions chemical ionization (PICI) have been employed to preserve the information on molecular ions and to improve specificity and sensitivity of quantitative determination.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Rosi L,Frediani P,Bartolucci Gdoi
10.1016/j.jpba.2012.10.006subject
Has Abstractpub_date
2013-02-23 00:00:00pages
31-8eissn
0731-7085issn
1873-264Xpii
S0731-7085(12)00546-8journal_volume
74pub_type
杂志文章abstract：:Substandard antimalarial drugs will result in unsatisfied therapeutic efficacy and increase the risk of resistance development. The point-of-care, qualitative, or semi-quantitative dipstick immunoassays cannot differentiate the substandard drugs with confidence. A rapid and quantitative analytical method that can be u...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113605
更新日期：2020-11-30 00:00:00
abstract：:The potentiometric response characteristics of diclofenac selective electrodes based on Fe(III) tetraphenylporphyrin-chloride (Fe(III)TPP-Cl) and Fe(III) tetrakis(pentafluorophenyl)porphyrin-chloride (Fe(III)TPFPP-Cl) in different mediator solvents and ionic additives are compared. The sensitivity, working range, dete...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.05.019
更新日期：2006-11-16 00:00:00
abstract：:Gastrodin is the major and bioactive component in Tianma (Gastrodia elata Bl.) and has sedative, anticonvulsive and neuroprotective effects. Since little is known about its neuropharmacokinetics and brain metabolism, this study was undertaken to investigate the kinetic inter-relationship of gastrodin in rat plasma, ce...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.10.017
更新日期：2008-01-22 00:00:00
abstract：:Isoniazid was subjected to different ICH prescribed stress conditions of thermal stress, hydrolysis, oxidation and photolysis. The drug was stable to dry heat (50 and 60 degrees C). It showed extensive decomposition under hydrolytic conditions, while it was only moderately sensitive to oxidation stress. The solid drug...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.10.013
更新日期：2007-03-12 00:00:00
abstract：:A stability study for amodiaquine (AQ) and desethylamodiaquine (AQm) in whole blood and plasma is reported. AQ, AQm and chloroquine (CQ) were simultaneously analysed and the ratios AQ/CQ and AQm/CQ were used to ensure correct interpretation of the stability results. CQ was stable in whole blood and plasma at all teste...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2005.10.018
更新日期：2006-04-11 00:00:00
abstract：:A simple, inexpensive and efficient sample preparation technique, three-phase hollow fiber liquid phase microextraction (HF-LPME), followed by high-performance liquid chromatography-ultra violet detection (HPLC-UV) was used for the analysis of warfarin in human plasma. Warfarin was extracted from 11.0 ml of aqueous so...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.11.019
更新日期：2012-03-05 00:00:00
abstract：:This paper deals with the chiral separation of optical isomers of beta-methyl-amino acids by CE and HPLC using the principle of ligand-exchange. Capillary zone electrophoresis was carried out using Cu(II) complexes of L-4-hydroxyproline (L-4-Hypro), N-(2-hydroxypropyl)-L-4-hydroxyproline (HP-L-4-Hypro) and N-(2-hydrox...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00616-1
更新日期：2002-01-15 00:00:00
abstract：:In recent years, thermal analysis has assumed major role in the pharmaceutical industry because it can be used to evaluate the stability both in the control of raw materials and the finished product, having employment potential in the development and characterization of new products and assessment processes. Tacrolimu...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.01.040
更新日期：2013-01-25 00:00:00
abstract：:The phytochemical research based on ethnopharmacology is considered an effective approach in the discovery of novel chemicals entities with potential as drug leads. Plants/plant extracts/decoctions, used by folklore traditions for treating several diseases, represent a source of chemical entities but no information ar...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2013.03.007
更新日期：2014-01-01 00:00:00
abstract：:A sensitive, rapid and selective liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed and validated for the simultaneous determination of baicalin, baicalein, wogonin, berberine, palmatine and jatrorrhizine in scutellaria-coptis herb couple in rat plasma. After protein precipitation with acet...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.04.002
更新日期：2010-11-02 00:00:00
abstract：:Two HPLC-UV methods are described for the separate determination of artemether (AM) and the combined preservatives, methylparaben and propylparaben in a pharmaceutical dosage form. These analytes are contained in a dry suspension with a high amount of non-soluble excipients, some of which can interfere with the analys...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.07.053
更新日期：2007-01-17 00:00:00
abstract：:Bepridil is potent inhibitor of Na+, K+ and Ca+ channel in cardiomyocytes. It has demonstrated strong antianginal effect with type I antiarrhythmic and with minimum antihypertensive therapeutic effect. Till date, a specific LC-MS/MS method to quantify Bepridil concentrations in biological matrix have not been reported...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.04.038
更新日期：2019-08-05 00:00:00
abstract：:Extracts from the Carica papaya L. plant are widely reported to contain metabolites with antibacterial, antioxidant and anticancer activity. This study aims to analyze the metabolic profiles of papaya leaves and seeds in order to gain insights into their phytomedicinal constituents. We performed metabolite fingerprint...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.06.035
更新日期：2015-11-10 00:00:00
abstract：:Polarography was the first developed automated method of voltage-controlled electrolysis with dropping mercury electrode (DME). Then, hanging mercury drop and static mercury drop electrodes were added as an alternative indicator electrode. In this way, polarography turned formally into voltammetry with mercury electro...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2016.05.006
更新日期：2016-10-25 00:00:00
abstract：:One of the major reasons for age-related cataract formation is an accumulation of insoluble lens proteins. In particular, higher-order α-crystallin aggregates, comprising αA and αB subunits, are insolubilized by the build up of various post-translational modifications over time. Although we previously found an excepti...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.06.017
更新日期：2015-12-10 00:00:00
abstract：:In situ ATR-FTIR spectroscopy was used as a screening method to quantify the relative release of pamidronate (PAM) from films of polyelectrolyte (PEL) complex (PEC) particles. Stable colloid PEC particles consisting of poly(ethyleneimine) (PEI) and cellulose sulphate (CS) loaded with PAM were obtained by PEL complexat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.03.047
更新日期：2012-07-01 00:00:00
abstract：:A reverse phase high performance liquid chromatographic method to determine tizanidine (TZ) and rofecoxib (RF) in combination is proposed and applied to the pharmaceuticals. This method allows the determination of 0.1-0.5 microg/ml of TZ and 1.2-6.0 microg/ml of RF along with 10 microg/ml of nimesulide (internal stand...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.09.039
更新日期：2005-02-07 00:00:00
abstract：:This study explores the potential of 177Lu-labeled carbon nanospheres as radio-nanoprobes for molecular imaging and therapy. The carboxyl functionalized surface of carbon nanospheres (CNS) was conjugated with [Gly-Gly-Gly-c(Asn-Gly-Arg)], G3-cNGR peptide through amide bond for targeting tumor vasculature and with [2-(...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.01.052
更新日期：2018-04-15 00:00:00
abstract：:The lignan (-)-grandisin has shown important pharmacological activities, such as citotoxicity and antiangiogenic, antibacterial and trypanocidal activities. So, it has been considered as a potential drug candidate. In the early drug development process, drug metabolism is one of the main parameters that should be eval...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.08.028
更新日期：2013-01-01 00:00:00
abstract：:A sensitive and specific LC-MS assay for DT-13 in rat plasma was developed. DT-13 is an active steroidal saponin present in Liriopes Radix and is developed as an anti-tumor drug candidate. The samples were extracted by acetonitrile-mediated plasma protein precipitation. The chromatographic separation was carried out u...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.07.003
更新日期：2011-11-01 00:00:00
abstract：:A simple, sensitive and rapid high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed and validated for the simultaneous quantitation of clopamide, reserpine and dihydroergotoxine (ergoloid mesylates) in human plasma. Under basic conditions, liquid-liquid extraction using ethy...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.03.051
更新日期：2016-06-05 00:00:00
abstract：:Mepitiostane (2α,3α-epithio-17β-(1-methoxycyclopentyloxy)-5α-androstane), which is a prodrug of epitiostanol (2α,3α-epitio-5α-androstane-17β-ol), is an epitiosteroid having anti-estrogenic and weak androgenic anabolic activities. The World Anti-Doping Agency prohibits the misuse of mepitiostane by athletes. Detection ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.07.016
更新日期：2015-11-10 00:00:00
abstract：:Surface plasmon resonance (SPR) is a promising tool in sensor technology for biomedical applications. An SPR based immunosensor was established for label free and real time assay for the serological diagnosis of dengue virus infection employing the dengue virus antigen as the sensing element. The dengue virus antigen ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.01.001
更新日期：2010-06-05 00:00:00
abstract：:Second derivative UV spectrophotometry proved to be a useful tool for the determination of acetaminophen, even in the presence of high amounts of the impurity, 4-aminophenol and the background effect caused by dissolved excipients of some dosage forms. The fluorimetric method used for the estimation of 4-aminophenol i...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(91)80051-a
更新日期：1991-01-01 00:00:00
abstract：:A rapid, sensitive and selective method for the determination of carvedilol in human plasma was developed using hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS). Carvedilol and cisapride (internal standard) were extracted from human plasma with methyl tert-butyl ether at basic ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.12.017
更新日期：2007-06-28 00:00:00
abstract：:A health supplement used for sexual performance enhancement was sent to Health Sciences Authority of Singapore for testing. An unknown compound was detected and isolated and its structure was elucidated using NMR, high-resolution MS, ESI-MS/MS, UV and IR. The compound, dapoxetine, is reported to be a selective seroton...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.06.005
更新日期：2009-12-05 00:00:00
abstract：:Current standards and regulations demand the pharmaceutical industry not only to produce highly pure drug substances, but to achieve a thorough understanding of the impurities accompanying their manufactured drug substances and products. These challenges have become important goals of process chemistry and have steadi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2014.04.016
更新日期：2014-12-01 00:00:00
abstract：:10 homeopathic remedies commercially available (each in 3 dilutions) as sugar granules, where half of them were of organic (and half inorganic) origin were subjected to solid-state infrared spectroscopy, both in middle infrared (ATR-FTIR) and near infrared (NIR) range. Measurements were repeated six times (six days, e...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.06.025
更新日期：2015-11-10 00:00:00
abstract：:The novel identification method for a heat-unstable antibiotic, FC/TA-891 and its active metabolite (FCE22101) by high-performance liquid chromatography (HPLC)-atmospheric pressure chemical ionization mass spectrometry (APCI-MS) employing bromoform as an ionization acceleration solvent, was applied to eight penicillin...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00402-8
更新日期：2002-11-07 00:00:00
abstract：:Phytochemical investigation of the methanolic extract of Byrsonima crassifolia's bark led to the isolation of 8 known phenolic compounds 5-O-galloylquinic acid, 3-O-galloylquinic acid, 3,4-di-O-galloylquinic acid, 3,5-di-O-galloylquinic acid, 3,4,5-tri-O-galloylquinic acid, (+)-epicatechin-3-gallate along with (+)-cat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.03.032
更新日期：2011-08-25 00:00:00
