Rapid Analysis of Halothane in Biological Samples using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry—A Case of a Double Homicide

Abstract

A simple, rapid, and sensitive method for the analysis of halothane in biological samples was developed. The procedure describes the extraction of halothane from blood, liver, kidney, brain, urine, bile, and stomach contents by headspace solid-phase microextraction (HS-SPME) followed by capillary gas chromatography coupled with mass spectrometry (GC-MS). The recovery in blood samples after addition of ammonium sulfate and sulfuric acid was 72% compared to a sample prepared in water (100%). Linearity was established over a concentration range of 0.1-100 mg/kg of spiked blood samples with an excellent coefficient of correlation (0.996) and a limit of detection of 0.004 mg/kg. The time for analysis was approximately 40 min per sample including the extraction step. The procedure was used for quantitation of halothane in various samples in a case of a double homicide. HS-SPME in combination with GC-MS was an effective method for the determination and quantitation of halothane in biological material.

Selected Ion Monitoring – Gas Chromatography/Mass Spectrometry Determination of Halothane Fumes in Operating Theatres

“…Even though the effect of chronic exposure to low concentrations of various anaesthetics is an issue of concern [10,11,18], no dose-response relationship has been reported in the literature for the health risks associated with occupational exposure [10]. Yet, public health authorities generally recommend threshold values [15,19,20] because halothane and related chemicals are known to accumulate in the organs of exposed personnel [14,21,22]. Exposure has been linked to multiple sclerosis [12], liver damage [5,9,11], DNA [14] and genotoxic effects [10,15].…”

“…Several analytical methods have been reported for the determination of halothane concentrations in air [19,20,[24][25][26], as well as in certain biological media: urine, blood, bile, liver and kidney [21]. There are a number of techniques that have been used for the detection and analysis of halothane, such as portable ambient air analysers provided with specific detectors [24], photoacoustic infrared spectroscopy [25,26], gas chromatography (GC) with FID [27] or ECD detector [19,20], and with coupled gas chromatography-mass spectrometry (GC-MS) [21]. For the chromatographic methods, halothane was collected prior to injection onto the chromatographic column through head-space solid phase micro-extraction from biological media [21], or by collection on active charcoal, followed by liquid extraction by benzyl-alcohol [19] or toluene [27].…”

Réponse analytique à une intoxication par substances volatiles

“…Dans le cas d'un double homicide suite à l'inhalation forcée de tissus imbibés d'halothane par les victimes, l'halothane a pu être identifié (22). Les concentrations mesurées par HS-CPG (7,2 mg/kg chez la femme de 82 ans et 3,0 mg/kg chez l'homme de 75 ans) étaient infé-rieures aux concentrations mortelles citées dans la littérature (7 à 720 mg/kg).…”

Qualitative screening for volatile organic compounds in human blood using solid‐phase microextraction and gas chromatography‐mass spectrometry

“…VOC are of great importance for forensic analytical toxicology. Volatile substance abuse is frequently fatal or can at least cause serious damage to health, often in conjunction with accidental autoerotic death 14–20. Furthermore, the investigation of burned bodies in consideration of fire accelerants can give information whether it was a case of accident or malicious arson and whether the victim was alive or not when the burning incident took place 21.…”