The Use of Fused-Silica Capillary Columns in Gas Chromatography and Gas Chromatography/Mass Spectrometry

1982 ◽  
pp. 118-132
Author(s):  
D. Meek ◽  
W. J. Reid
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Capillary Columns ◽  
Fused Silica ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Fused Silica Capillary ◽  
Fused Silica Capillary Columns ◽  
Silica Capillary

Postmortem Analysis of Benzodiazepines in Human Bone by Gas Chromatography–Mass Spectrometry

2020 ◽  
Author(s):  
Rosanna Mancini ◽  
Lucia Fernadez-Lopez ◽  
Maria Falcon ◽  
Manuela Pellegrini ◽  
Aurelio Luna ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Fused Silica ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Fused Silica Capillary ◽  
Silica Capillary Column

Abstract A procedure based on gas chromatography-mass spectrometry was developed for the analysis of benzodiazepines (nordiazepam, oxazepam, lormetazepam, lorazepam, clonazepam, bromazepam and alprazolam) in postmortem human ribs. Powdered bone samples, including marrow remains inside, with the internal standard diazepam-d5 were subjected to enzymatic hydrolysis with 100 μL of β-glucoronidase and were incubated in sodium hydroxide for 1 h in a 70°C oven. Samples underwent liquid phase extraction and ethyl acetate was used as eluent. Chromatography was performed on a fused silica capillary column and the selected-ion-monitoring mode was used for analytes determination. The method was validated in the range 0.1–0.5 ng/mg (depending on the benzodiazepine) to 100 ng/mg with average values of recovery, matrix effect and process efficiency ranged from 83.2 to 94.3%, from 97.3 to 102.1% and from 80.5 to 91.2%, respectively. The intra- and inter-day accuracy was <15%. The procedure was tested in rib specimens obtained during routine autopsies from 20 cases where these benzodiazepines were found in blood. Benzodiazepines were detected in the combined bone and marrow samples in 60% of cases. Lorazepam was detected in bone in the range of 0.3–0.7 ng/mg, nordiazepam at 1.3–4.2 ng/mg and oxazepam at 1.1–1.2 ng/mg. To our knowledge, this protocol for the simultaneous analysis of these benzodiazepines is the first performed and validated using human ribs.

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