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Predicate | Object |
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rdf:type | |
lifeskim:mentions | |
pubmed:issue |
6
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pubmed:dateCreated |
1995-2-3
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pubmed:abstractText |
Effective solid-phase extraction, derivatization, and GC/MS procedures are developed for the simultaneous determinations of butalbital, amobarbital, pentobarbital, and secobarbital, using a deuterated pentobarbital (d5-pentobarbital) as the internal standard. Buffered (pH 7) urine samples were extracted with Bond Elute Certify II cartridge. Iodomethane/tetramethylammonium hydroxide in dimethylsulfoxide was used for methylation, while a HP 5970 MSD equipped with a 13 m J & W DB-5 column (5% phenyl polysiloxane phase) and the Thru-Put Target software package were used for GC/MS analysis and data processing. This protocol was found to be superior, in both chromatographic performance characteristics and quantitation results, over a liquid-liquid extraction procedure without derivatization using hexobarbital as the internal standard. Extraction recoveries observed from control samples containing four barbiturates range from 80% to 90%. Good one-point calibration data are obtained for all four barbiturates in the 50 to 3200 ng/mL range. Interestingly, the one-point calibration data for pentobarbital are inferior to the other three barbiturates--due to interference from the internal standard (d5-pentobarbital). The calibration data of pentobarbital are best described by a hyperbolic curve regression model. Precision data (% CV) for GC/MS analysis, over-all procedure, and day-to-day performance are approximately 2.0%, 6.0%, and 8.0%, respectively. With the use of a 2 mL sample size, the attainable detection limit is approximately 20 ng/mL.
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pubmed:language |
eng
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pubmed:journal | |
pubmed:citationSubset |
IM
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pubmed:chemical |
http://linkedlifedata.com/resource/pubmed/chemical/Amobarbital,
http://linkedlifedata.com/resource/pubmed/chemical/Barbiturates,
http://linkedlifedata.com/resource/pubmed/chemical/Pentobarbital,
http://linkedlifedata.com/resource/pubmed/chemical/Secobarbital,
http://linkedlifedata.com/resource/pubmed/chemical/butalbital
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pubmed:status |
MEDLINE
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pubmed:month |
Nov
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pubmed:issn |
0022-1198
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pubmed:author | |
pubmed:issnType |
Print
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pubmed:volume |
39
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pubmed:owner |
NLM
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pubmed:authorsComplete |
Y
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pubmed:pagination |
1504-14
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pubmed:dateRevised |
2006-11-15
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pubmed:meshHeading |
pubmed-meshheading:7815030-Amobarbital,
pubmed-meshheading:7815030-Barbiturates,
pubmed-meshheading:7815030-Calibration,
pubmed-meshheading:7815030-Gas Chromatography-Mass Spectrometry,
pubmed-meshheading:7815030-Humans,
pubmed-meshheading:7815030-Methylation,
pubmed-meshheading:7815030-Pentobarbital,
pubmed-meshheading:7815030-Reproducibility of Results,
pubmed-meshheading:7815030-Secobarbital
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pubmed:year |
1994
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pubmed:articleTitle |
Improved gas chromatography/mass spectrometry analysis of barbiturates in urine using centrifuge-based solid-phase extraction, methylation, with d5-pentobarbital as internal standard.
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pubmed:affiliation |
Department of Criminal Justice, University of Alabama at Birmingham.
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pubmed:publicationType |
Journal Article
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