RESUMEN
ABSTRACT: Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry ï¼UPLC-MS/MSï¼ rapid determination method for simultaneous analysis of 20 fentanyl-related substances in blood. Methods With fentanyl-D5 as an internal standard, the blood was extracted by liquid-liquid extraction ï¼LLEï¼, then separated with an ACQUITY UPLC HSS T3 chromatographic column, and finally 20 fentanyl-related substances were simultaneously analyzed with multiple reaction monitoring ï¼MRMï¼ mode. Results The limits of detection ï¼LODï¼ of all compounds were 0.02-0.03 ng/mL, and the limits of quantitation ï¼LOQï¼ were 0.05-0.2 ng/mL. Within the mass concentration range of 0.05-40 ng/mL, 20 fentanyl-related substances had a good linear relationship, and correlation coefficients were larger than 0.99. The accuracy of the method was 87.69%-114.68% and the extraction recovery rate was 85.35%-101.80%, and no significant matrix effect was observed. The established method was successfully applied to the detection of sufentanil in rat blood after sufentanil was injected. Sufentanil could still be detected in blood of rats 10 h after sufentanil injection. Conclusion The established method has the advantages of simple pretreatment, high sensitivity and good selectivity, and can be used for the determination of fentanyl-related substances in forensic toxicology analysis.
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Cromatografía Líquida de Alta Presión , Fentanilo/sangre , Espectrometría de Masas en Tándem , Animales , Toxicología Forense , Ratas , Reproducibilidad de los Resultados , Sufentanilo/sangreRESUMEN
OBJECTIVES: To establish a rapid determination method with LC-MS/MS for cocaine and its metabolite benzoylecgonine in hair. METHODS: Deuterated internal standards ï¼cocaine-D3 and benzoylecgonine-D8ï¼ were added to the decontaminated hair. After the extraction by ultrasonication with methanol, the compounds were separated by the Restek Allure PFP propyl column, and cocaine and benzoylecgonine were simultaneously analysed in multiple reaction monitoring mode. RESULTS: The cocaine and benzoylecgonine in hair showed a good linearity in the range of mass fraction between 0.02 and 10.00 ng/mg with the limits of detection of 0.01 ng/mg. CONCLUSIONS: The developed method is simple and rapid with a good selectivity, which is suitable for the determination of cocaine and its metabolite benzoylecgonine in hair.
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Cromatografía Liquida/métodos , Cocaína/análogos & derivados , Cocaína/análisis , Cabello/química , Espectrometría de Masas en Tándem/métodos , Cromatografía Líquida de Alta Presión , Cocaína/administración & dosificación , Cocaína/metabolismo , Cabello/metabolismo , Humanos , Estándares de Referencia , Reproducibilidad de los ResultadosRESUMEN
OBJECTIVES: To establish a gas chromatography-mass spectrometry ï¼GC-MSï¼ method for the determination of sulfide ion in blood and apply it to the practical cases. METHODS: The 1, 3, 5-tribromobenzene was selected as an internal standard, and 0.2 mL blood sample was collected and analyzed using GC-MS after α-Bromo-2, 3, 4, 5, 6-pentafluorobenzyl bromide derivatization. RESULTS: The mass concentration of sulfide ion in blood had good linearity in the range of 0.2-40 µg/mL with a limit of detection ï¼LODï¼ of 0.05 µg/mL. The mass concentration of sulfide ion was less than 0.05 µg/mL in blank blood from different sources such as healthy subjects and dead cases. In 3 sulfide poisoning cases, sulfide ion was detected in the blood samples of 6 victims, and the mass concentration range was 1.02-3.13 µg/mL. CONCLUSIONS: This study establishes a method for investigation of sulfide ion in blood which has been applied successfully to the cases of fatal sulfide poisonings.