Online citations, reference lists, and bibliographies.

Simultaneous Determination Of Multibenzodiazepines By HPLC/UV: Investigation Of Liquid-liquid And Solid-phase Extractions In Human Plasma.

K. Borges, Ellen Figueiredo Freire, Isarita Martins, M. D. de Siqueira
Published 2009 · Chemistry, Medicine

Cite This
Download PDF
Analyze on Scholarcy
Share
A method for simultaneous determination of seven benzodiazepines (BZPs) (flunitrazepam, clonazepam, oxazepam, lorazepam, chlordiazepoxide, nordiazepam and diazepam using N-desalkylflurazepam as internal standard) in human plasma using liquid-liquid and solid-phase extractions followed by high-performance liquid chromatography (HPLC) is described. The analytes were separated employing a LC-18 DB column (250 mm x 4.6 mm, 5 microm) at 35 degrees C under isocratic conditions using 5mM KH(2)PO(4) buffer solution pH 6.0:methanol:diethyl ether (55:40:5, v/v/v) as mobile phase at a flow rate of 0.8 mL min(-1). UV detection was carried out at 245 nm. Employing LLE, the best conditions were achieved with double extraction of 0.5 mL plasma using ethyl acetate and Na(2)HPO(4) pH 9.5 for pH adjusting. Employing SPE, the best conditions were achieved with 0.5 mL plasma plus 3 mL 0.1M borate buffer pH 9.5, which were then passed through a C18 cartridge previously conditioned, washed for 3 times with these solvents: 3 mL 0.1M borate buffer pH 9.5, 4 mL Milli-Q water and 1 mL acetonitrile 5%, finally the BZPs elution was carried with diethyl ether:n-hexane:methanol (50:30:20). In both methods the solvent was evaporated at 40 degrees C under nitrogen flow. The validation parameters obtained in LLE were linearity range of 50-1200 ng mL(-1) plasma (r>or=0.9927), limits of quantification of 50 ng mL(-1) plasma, within-day and between-day CV% and E% for precision and accuracy lower than 15%, and recovery above 65% for all BZPs. In SPE, the parameter obtained were linearity range of 30-1200 ng mL(-1) plasma (r>or=0.9900), limits of quantification of 30 ng mL(-1) plasma, within-day and between-day CV% and E% for precision and accuracy lower than 15% and recovery above 55% for all BZPs. These extracting procedures followed by HPLC analysis showed their suitable applicability in order to examine one or more BZPs in human plasma. Moreover, it could be suggested that these procedures might be employed in various analytical applications, in special for toxicological/forensic analysis.
This paper references
10.1016/S0731-7085(03)00426-6
Direct injection HPLC method for the determination of selected benzodiazepines in plasma using a Hisep column.
C. Pistos (2003)
10.1016/S0731-7085(01)00461-7
Direct LC analysis of five benzodiazepines in human urine and plasma using an ADS restricted access extraction column.
W. Mullett (2001)
10.1016/0731-7085(93)80187-6
The determination of bromazepam in plasma by reversed-phase high-performance liquid chromatography.
H. Le Solleu (1993)
10.1039/AN9749900241
The determination of some 1,4-benzodiazepines and their metabolites in body fluids. A review.
J. Clifford (1974)
10.1520/JFS10938J
Postmortem behavior of serum thyroxine, triiodothyronine, and parathormone.
E. Rachut (1980)
10.1016/S0021-9673(00)00806-2
Selective and sensitive assay for the determination of benzodiazepines by high-performance liquid chromatography with simultaneous ultraviolet and reductive electrochemical detection at the hanging mercury drop electrode.
M. Wilhelm (2000)
10.1016/0731-7085(94)00070-0
A selective fluorimetric method for the determination of some 1,4-benzodiazepine drugs containing a hydroxyl group at C-3.
M. Walash (1994)
Anal
A. A. Salem (2003)
10.1093/clinchem/30.10.1652
Quantification of alprazolam in serum or plasma by liquid chromatography.
S. R. Mccormick (1984)
10.1016/J.CHROMA.2003.08.068
Monitoring of drugs and metabolites in whole blood by restricted-access solid-phase microextraction coupled to liquid chromatography-mass spectrometry.
M. Walles (2004)
10.1039/an9840900813
Determination of clobazam and desmethylclobazam in serum using high-performance liquid chromatography.
N. Ratnaraj (1984)
10.1016/J.JCHROMB.2006.01.009
A fast LC-APCI/MS method for analyzing benzodiazepines in whole blood using monolithic support.
Aurélie Bugey (2006)
10.1016/0379-0738(92)90081-7
Quantitative liquid chromatography, thermospray/tandem mass spectrometry (LC/TSP/MS/MS) analysis of some thermolabile benzodiazepines in whole-blood.
A. M. Verweij (1992)
10.1016/S0379-0738(96)02063-4
Detection of alprazolam in hair by negative ion chemical ionization mass spectrometry.
K. Höld (1997)
10.1016/0731-7085(92)80033-J
Dialysis as an on-line sample-pretreatment technique for column liquid chromatography: influence of experimental variables upon the determination of benzodiazepines in human plasma.
N. C. van de Merbel (1992)
Biomed
R. S. Guerrero (1993)
10.1016/0731-7085(93)80126-L
On-line photoreaction and fluorimetric determination of diazepam
R. S. Guerrero (1993)
Spectrochim
A. A. Salem (2004)
10.1016/J.JPBA.2004.01.023
Rapid analysis of benzodiazepines in whole blood by high-performance liquid chromatography: use of a monolithic column.
Aurélie Bugey (2004)
Chem
A. A. Salem (2009)
10.1093/clinchem/28.11.2274
Liquid-chromatographic procedure for simultaneous analysis for eight benzodiazepines in serum.
G. Lensmeyer (1982)
10.1016/0039-9140(95)01772-0
High performance liquid chromatographic method for the separation and quantification of some psychotherapeutic benzodiazepines optimized by the modified simplex procedure.
S. M. Sultan (1996)
10.1016/0379-0738(90)90269-5
The determination of drugs of abuse in whole blood by means of FPIA and EMIT-dau immunoassays--a comparative study.
M. Bogusz (1990)
10.1016/S0003-2670(03)00304-0
Simple method for the determination of benzodiazepines in human body fluids by high-performance liquid chromatography–mass spectrometry
X. Lee (2003)
10.1016/S0021-9673(01)83413-0
Diazepam metabolism during chronic medication unbound fraction in plasma, erythrocytes and urine.
I. Zingales (1973)
10.1016/0731-7085(95)01703-8
Automated on-line dialysis for sample preparation for gas chromatography: determination of benzodiazepines in human plasma.
R. Herráez-Hernández (1996)
10.1016/J.JCHROMB.2004.12.038
Liquid chromatography-electrospray ionisation mass spectrometry for the determination of nine selected benzodiazepines in human plasma and oral fluid.
Ó. Quintela (2005)
10.1016/J.FORSCIINT.2004.04.066
Determination of bromazepam, clonazepam and metabolites after a single intake in urine and hair by LC-MS/MS. Application to forensic cases of drug facilitated crimes.
M. Chèze (2004)
10.1016/0731-7085(92)80046-P
Simultaneous determination of common benzodiazepines in blood using capillary gas chromatography.
H. Gjerde (1992)
10.1016/S0021-9673(99)00236-8
Determination of 1,4-benzodiazepines and their metabolites by capillary electrophoresis and high-performance liquid chromatography using ultraviolet and electrospray ionisation mass spectrometry.
S. McClean (1999)
10.1016/J.JCHROMB.2004.03.079
Quantitative analysis of 33 benzodiazepines, metabolites and benzodiazepine-like substances in whole blood by liquid chromatography-(tandem) mass spectrometry.
B. Smink (2004)
10.1515/9783111576855-015
J
Seguin Hen (1824)
10.1016/J.JCHROMB.2004.12.032
Determination of 14 benzodiazepines and hydroxy metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography-mass spectrometry.
Teemu Gunnar (2005)
10.1016/S0379-0738(00)00226-7
Screening and determination of benzodiazepines in whole blood using solid-phase extraction and gas chromatography/mass spectrometry.
H. Inoue (2000)
10.1002/0471463728.CH8
Bioanalytical Method Validation
F. Garofolo (2004)
10.1590/S0100-40422005000500007
Diazepam e nordiazepam em plasma: métodos de extração líquido-líquido e em fase sólida no pré-tratamento de amostras para análise cromatográfica em fase líquida
Ellen Figueiredo Freire (2005)
10.1016/S0731-7085(00)00325-3
Simultaneous determination of benzodiazepines in whole blood or serum by HPLC/DAD with a semi-micro column.
A. El Mahjoub (2000)
10.1016/S0378-4347(01)00419-4
Simultaneous determination of fifteen low-dosed benzodiazepines in human urine by solid-phase extraction and gas chromatography-mass spectrometry.
D. Borrey (2001)
10.1016/S0021-9673(01)89184-6
Trace analysis of benzodiazepine drugs in blood using deactivated amberlite XAD-7 porous polymer beads and silica capillary column gas chromatography with electron-capture detection.
J. Douse (1984)
Biomed
M. I. Walash (1994)
Forensic Sci
M. Bogusz (1990)
10.1016/S0731-7085(98)00275-1
Determination of benzodiazepines in human urine and plasma with solvent modified solid phase micro extraction and gas chromatography; rationalisation of method development using experimental design strategies.
K. J. Reubsaet (1998)
10.1016/J.ACA.2003.08.070
Potentiometric determination of diazepam, bromazepam and clonazepam using solid contact ion-selective electrodes
A. Salem (2003)
10.1016/S0379-0738(01)00511-4
Determination of benzodiazepines in human hair by on-line high-performance liquid chromatography using a restricted access extraction column.
A. El Mahjoub (2001)
10.1016/S0021-9673(02)00216-9
Bio-compatible in-tube solid-phase microextraction capillary for the direct extraction and high-performance liquid chromatographic determination of drugs in human serum.
W. Mullett (2002)
10.1016/S0731-7085(02)00520-4
Determination of hypnotic benzodiazepines (alprazolam, estazolam, and midazolam) and their metabolites in rat hair and plasma by reversed-phase liquid-chromatography with electrospray ionization mass spectrometry.
T. Toyo’oka (2003)
Forensic Sci
A.M.A. Verweij (1992)



This paper is referenced by
10.1080/00032719.2017.1316729
Graphene-modified Monolithic Capillary Column for the Microextraction of Trace Benzodiazepines in Biological Samples
Weixuan Yao (2017)
10.1002/bmc.3615
Simplifying sample preparation using fabric phase sorptive extraction technique for the determination of benzodiazepines in blood serum by high-performance liquid chromatography.
V. Samanidou (2016)
10.1016/j.chroma.2014.04.067
Development of a new microextraction method based on elevated temperature dispersive liquid-liquid microextraction for determination of triazole pesticides residues in honey by gas chromatography-nitrogen phosphorus detection.
M. Mogaddam (2014)
10.1039/c9nj05196a
Metal organic framework/chitosan foams functionalized with polyethylene oxide as a sorbent for enrichment and analysis of bisphenols in beverages and water
Shuo Li (2020)
10.1080/03067319.2020.1773453
Application of temperature-assisted tandem dispersive liquid–liquid microextraction for the extraction and high preconcentration of triazole pesticides
Mohammad Reza Afshar Mogaddam (2020)
10.1002/jssc.201600010
Preconcentration of valsartan by dispersive liquid-liquid microextraction based on solidification of floating organic drop and its determination in urine sample: Central composite design.
Arezou Amiri Pebdani (2016)
10.1111/j.1472-8206.2009.00788.x
Anxiolytic‐like effect of Carvacrol (5‐isopropyl‐2‐methylphenol) in mice: involvement with GABAergic transmission
F. H. Melo (2010)
10.1002/jssc.201501273
Preparation of a novel sorptive stir bar based on vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma.
Mahsa Torabizadeh (2016)
10.1007/s13738-016-1003-y
Determination of migrated phthalic acid residues into edible oils using a green mode of air-assisted liquid–liquid microextraction followed by high-performance liquid chromatography–diode array detector
Mir Ali Farajzadeh (2016)
10.1016/j.chroma.2009.11.026
Solid drop based liquid-phase microextraction.
Mohammad Reza Ganjali (2010)
10.1039/C6RA22353B
Magnetic zinc oxide nanoflower-assisted ionic liquid-based nanofluid dispersive liquid–liquid microextraction for the rapid determination of acaricides in tea infusions
Miyi Yang (2016)
10.1007/s13738-016-0939-2
Application of dispersive liquid–liquid microextraction followed by gas chromatography/mass spectrometry as effective tool for trace analysis of organochlorine pesticide residues in honey samples
M Mousavi (2016)
10.4236/AJAC.2012.32017
Fast Determination of Benzodiazepines in Human Urine via Liquid-Liquid Extraction with Low Temperature Partitioning and LC-HRMS
Elisângela Jaqueline Magalhães (2012)
10.1155/2015/293719
Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities
Rania N. El-Shaheny (2015)
10.1016/j.jfca.2019.103315
An analytical strategy for propoxur determination in raisin samples with matrix matching method after dispersive liquid-liquid microextraction
Tülay Borahan (2019)
10.1556/ACHROM.23.2011.2.5
Identification and determination of compounds belonging to the group of OUN pharmaceutical agents by thin-layer chromatography with densitometric detection in biological material
Anna Maślanka (2011)
10.1039/C6RA15981H
Application of Ni:ZnS nanoparticles loaded on magnetic multi-walled carbon nanotubes as a sorbent for dispersive micro-solid phase extraction of phenobarbital and phenytoin prior to HPLC analysis: experimental design
A. A. Pebdani (2016)
10.1016/j.foodchem.2016.05.157
Application of elevated temperature-dispersive liquid-liquid microextraction for determination of organophosphorus pesticides residues in aqueous samples followed by gas chromatography-flame ionization detection.
M. A. Farajzadeh (2016)
10.1016/j.legalmed.2016.11.005
Rapid and highly sensitive analysis of benzodiazepines and tandospirone in human plasma by automated on-line column-switching UFLC-MS/MS.
Xiao-Pen Lee (2017)
10.1002/jssc.201900373
Synthesis of mesoporous silica for adsorption of chlordiazepoxide and its determination by HPLC: Experimental design.
Fatemeh Momtazan (2019)
10.1016/j.talanta.2009.08.033
Quantitation of atorvastatin in human plasma using directly suspended acceptor droplet in liquid-liquid-liquid microextraction and high-performance liquid chromatography-ultraviolet detection.
Hadi Farahani (2009)
10.1016/j.talanta.2015.08.014
Preparation of magnetic graphene @polydopamine @Zr-MOF material for the extraction and analysis of bisphenols in water samples.
Xianying Wang (2015)
10.1016/j.talanta.2009.04.069
Chromatographic retention prediction and octanol-water partition coefficient determination of monobasic weak acidic compounds in ion-suppression reversed-phase liquid chromatography using acids as ion-suppressors.
X. Ming (2009)
10.1016/j.saa.2015.03.057
Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.
Arezou Amiri Pebdani (2015)
10.4155/bio.10.174
Young investigator.
Keyller Bastos Borges (2011)
10.1002/jssc.201500743
Superparamagnetic Fe3 O4 @SiO2 core-shell composite nanoparticles for the mixed hemimicelle solid-phase extraction of benzodiazepines from hair and wastewater samples before high-performance liquid chromatography analysis.
Effat Esmaeili-Shahri (2015)
Simultaneous Determination of Six Benzodiazepines in Spiked Soft Drinks by High Performance Liquid Chromatography with Ultra Violet Detection (HPLC-UV)
Kambiz Soltaninejad (2016)
10.1080/00032719.2011.582554
Determination of Diazepam and Nordiazepam in the Plasma of Psychiatric Patients in Long-Term Treatment Employing Liquid-Liquid and Solid Phase Extraction by Gas Chromatography with Electron Capture Detection
Keyller Bastos Borges (2011)
10.1039/C4AY01348D
Optimization of ultrasound-assisted dispersive liquid–liquid microextraction for ultra performance liquid chromatography determination of benzodiazepines in urine and hospital wastewater
Purificación Fernández (2014)
10.1016/j.jpba.2015.02.017
Analytical methodologies for the determination of benzodiazepines in biological samples.
Karolina Persona (2015)
10.1016/j.jchromb.2015.11.043
Preconcentration and determination of chlordiazepoxide and diazepam drugs using dispersive nanomaterial-ultrasound assisted microextraction method followed by high performance liquid chromatography.
Arezou Amiri Pebdani (2016)
10.1002/jssc.201201069
Mixed-mode SPE for a multi-residue analysis of benzodiazepines in whole blood using rapid GC with negative-ion chemical ionization MS.
Nerijus Karlonas (2013)
See more
Semantic Scholar Logo Some data provided by SemanticScholar