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A validated method for simultaneous screening and quantification of twenty-three benzodiazepines and metabolites plus zopiclone and zaleplone in whole blood by liquid-liquid extraction and ultra-performance liquid chromatography- tandem mass spectrometry.
- Source :
-
Journal of analytical toxicology [J Anal Toxicol] 2010 Jul-Aug; Vol. 34 (6), pp. 332-41. - Publication Year :
- 2010
-
Abstract
- An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for detection of 23 benzodiazepines and related compounds in whole blood was developed and validated. The method is used for screening and quantitation of benzodiazepines in whole blood received from autopsy cases and living persons. The detected compounds were alprazolam, bromazepam, brotizolam, chlordiazepoxide, demoxepam, clobazam, clonazepam, 7-aminoclonazepam, diazepam, nordiazepam, estazolam, flunitrazepam, 7-aminoflunitrazepam, lorazepam, lormetazepam, midazolam, nitrazepam, 7-aminonitrazepam, oxazepam, temazepam, triazolam, zaleplon, and zopiclone. Whole blood from drug-free volunteers was used for all experiments. Blood samples (0.200 g) were extracted with ethyl acetate at pH 9. Target drugs were quantified using a Waters ACQUITY UPLC system coupled to a Waters Quattro Premier XE triple quadrupole in positive electrospray ionization, multiple reaction monitoring mode. The use of deuterated internal standards for most compounds verified that the accuracy of the method was not influenced by matrix effects. Extraction recoveries were 73-108% for all analytes. Lower limits of quantification ranged from 0.002 to 0.005 mg/kg. Long-term imprecision (CV%) ranged from 6.0 to 18.7%. We present a fully validated UPLC-MS-MS method for 23 benzodiazepines in whole blood with a run-time of only 5 min and using only 0.200 g of whole blood.
- Subjects :
- Acetamides isolation & purification
Azabicyclo Compounds isolation & purification
Benzodiazepines isolation & purification
Humans
Piperazines isolation & purification
Pyrimidines isolation & purification
Acetamides blood
Azabicyclo Compounds blood
Benzodiazepines blood
Chromatography, Liquid
Piperazines blood
Pyrimidines blood
Substance Abuse Detection methods
Tandem Mass Spectrometry
Subjects
Details
- Language :
- English
- ISSN :
- 1945-2403
- Volume :
- 34
- Issue :
- 6
- Database :
- MEDLINE
- Journal :
- Journal of analytical toxicology
- Publication Type :
- Academic Journal
- Accession number :
- 20663286
- Full Text :
- https://doi.org/10.1093/jat/34.6.332