Development and validation of a GC/MS method for the determination of buprenorphine and norbuprenorphine in blood

Papoutsis, Ioannis; Nikolaou, Panagiota; Athanaselis, Sotirios; Pistos, Constantinos; Spiliopoulou, Chara; Maravelias, C

doi:10.1016/j.toxlet.2009.06.395

Cited by 4 publications

(4 citation statements)

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“…In Table are compared the figures of merits for the determination of chlordiazepoxide in various in urine samples by the proposed DLLME‐HPLC‐UV with those of the previously published methods. The proposed method in all matrices has the wide linearity range and low LOD. Therefore the proposed analytical method can be used for determination of chlordiazepoxide in different matrices.…”

Section: Resultsmentioning

confidence: 99%

Optimization of dispersive liquid-liquid microextraction with central composite design for preconcentration of chlordiazepoxide drug and its determination by HPLC-UV

Khodadoust

Ghaedi

2013

J. Sep. Science

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A simple, rapid, and sensitive method based on dispersive liquid-liquid microextraction combined with HPLC-UV detection applied for the quantification of chlordiazepoxide in some real samples. The effect of different extraction conditions on the extraction efficiency of the chlordiazepoxide drug was investigated and optimized using central composite design as a conventional efficient tool. Optimum extraction condition values of variables were set as 210 μL chloroform, 1.8 mL methanol, 1.0 min extraction time, 5.0 min centrifugation at 5000 rpm min(-1), neutral pH, 7.0% w/v NaCl. The separation was reached in less than 8.0 min using a C18 column using isocratic binary mobile phase (acetonitrile/water (60:40, v/v)) with flow rate of 1.0 mL min(-1) The linear response (r(2) > 0.998) was achieved in the range of 0.005-10 μg mL(-1) with detection limit 0.0005 μg mL(-1) The applicability of this method for simultaneous extraction and determination of chlordiazepoxide in four different matrices (water, urine, plasma, and chlordiazepoxide tablet) were investigated using standard addition method. Average recoveries at two spiking levels were over the range of 91.3-102.5% with RSD < 5.0% (n = 3). The obtained results show that dispersive liquid-liquid microextraction combined with HPLC-UV is a fast and simple method for the determination of chlordiazepoxide in real samples.

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Section: Resultsmentioning

confidence: 99%

Optimization of dispersive liquid-liquid microextraction with central composite design for preconcentration of chlordiazepoxide drug and its determination by HPLC-UV

Khodadoust

Ghaedi

2013

J. Sep. Science

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“…Many methods reported in literature are focused on the determination of BDZ in the biological tissues of the victim, i.e. blood, hair, and urine . In many cases, the violence is reported to the police with a considerable time delay .…”

Section: Introductionmentioning

confidence: 99%

Liquid chromatography-electron ionization tandem mass spectrometry with the Direct-EI interface in the fast determination of diazepam and flunitrazepam in alcoholic beverages

2016

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This is the first application based on electron ionization (EI) using a Direct-EI LC interface and MS/MS to detect unequivocally target compounds in a very small real sample. The determination and quantification of benzodiazepines in very small residues of beverages, collected at the scene of drug-facilitated crimes are mandatory in legal procedures. A specific and sensitive analytical instrumentation is needed, involving little or no sample preparation. Here, a direct flow injection analysis of alcoholic beverages spiked with commercially available drugs containing diazepam and flunitrazepam is presented. The method proposed is very fast and requires neither sample preparation nor chromatographic separation. Linearity (R(2) ) was between 0.9977 and 0.9992; LOD and LOQ spanned from 0.01 to 0.02 ng/μL and from 0.1 to 0.5 ng/μL, respectively; intra- and interday repeatabilities were between 1 and 8%. No matrix effects were observed from the comparison of the linear regression curves obtained in real fortified samples and in pure ethanol. Vodka, whisky, and white wine specimens were fortified with commercial drugs, Valium(®) and Rohypnol(®) , at two different concentrations (20 and 50 ng/μL) to simulate the typical amounts found in adulterated real samples and analyzed to demonstrate the method applicability to forensic analyses.

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“…Several analytical methods have been employed to determine the concentration of benzodiazepines in blood and plasma including HPLC , LC‐MS/MS , and finally GC/MS using electron impact (GC/EI‐MS) or electron capture ionization techniques . Gas chromatography with negative ion chemical ionization (GC/NICI‐MS) is a sensitive and selective technique for the analysis of benzodiazepines.…”

Section: Introductionmentioning

confidence: 99%

“…Furthermore, the low therapeutic concentrations of benzodiazepines request a highly sensitive method for their determination. However, the sensitivities of the most currently used methods do not meet this requirement .…”

Section: Introductionmentioning

confidence: 99%

Mixed‐mode SPE for a multi‐residue analysis of benzodiazepines in whole blood using rapid GC with negative‐ion chemical ionization MS

Karlonas

Padarauskas

Ramanavičius

et al. 2013

J of Separation Science

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A sensitive and selective method for simultaneous quantitation of 15 benzodiazepines in human whole blood using rapid GC with negative-ion chemical ionization MS is proposed. A mixed-mode cation-exchange polymeric sorbent was used for SPE. Different extraction solvents or mixtures of solvents of different compositions for elution of the adsorbed analytes, and washing steps for eliminating interferences in the column were tested. Analytes were eluted from the column using 5% v/v NH4 OH in methanol. A derivatization step using different silylation reagents, time, and temperature was tested. Extracts from SPE were silylated by a mixture of N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide, acetonitrile, ethyl acetate, and subjected to gas chromatographic analysis. The LODs of 15 benzodiazepines in whole blood samples ranged from 0.24-0.62 ng mL(-1). The RSDs of samples used for three different quality control concentration levels were lower than 7.0%, and the accuracy ranged from 89.5 to 110.5%. The results show that the developed method is accurate, sensitive, selective, and very fast. Finally, the applicability of this method for determination of trace concentrations of several benzodiazepines in real blood samples has been demonstrated.

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Development and validation of a GC/MS method for the determination of buprenorphine and norbuprenorphine in blood

Cited by 4 publications

References 0 publications

Optimization of dispersive liquid-liquid microextraction with central composite design for preconcentration of chlordiazepoxide drug and its determination by HPLC-UV

Optimization of dispersive liquid-liquid microextraction with central composite design for preconcentration of chlordiazepoxide drug and its determination by HPLC-UV

Liquid chromatography-electron ionization tandem mass spectrometry with the Direct-EI interface in the fast determination of diazepam and flunitrazepam in alcoholic beverages

Mixed‐mode SPE for a multi‐residue analysis of benzodiazepines in whole blood using rapid GC with negative‐ion chemical ionization MS

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