RESUMO
OBJECTIVE: To develop a method of SPE-LC-MS/MS for the determination of doxepin in whole blood. METHODS: After solid phase extraction, the samples were identified by LC-MS/MS. Positive ion electrospray ionization mode and multiple reaction monitoring (MRM) mode was selected. Amitriptyline was used as internal standard. The m/z of doxepin: 280-->107, 280-->235 and 280-->220. The m/z of amitriptyline: 278-->233. The retaining time of doxepin and amitriptyline were 15.15 and 16.94 min, respectively. RESULTS: The calibration curve was linear among the concentration of doxepin range from 0.005 to 1.00 microg/mL. The linear correlation equation was y = 3.2047x + 0.0339, the correlation coefficient was 0.9996. The detection limit of doxepin was 0.001 microg/mL and average recovery rate was 78.0%-82.9%. The relative standard precision for within-day and between-day were less than 2.55% and 5.90%, respectively. CONCLUSION: The method is effective, simple, reliable and can be used in the determination of doxepin in whole blood.
Assuntos
Antidepressivos Tricíclicos/sangue , Cromatografia Líquida/métodos , Doxepina/sangue , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Amitriptilina/sangue , Antidepressivos Tricíclicos/intoxicação , Biomarcadores/análise , Biomarcadores/sangue , Doxepina/intoxicação , Overdose de Drogas , Toxicologia Forense , Humanos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrometria de Massas por Ionização por ElectrosprayRESUMO
OBJECTIVE: To develop a method to measure trihexyphenidyl, chlorpromazine and clozapine in human blood with GC-MS. METHODS: The specimens were alkalized (pH > 10) and extracted with V (benzene):V(ethyl acetate) = 1:1, and qualitatively analyzed using GC-MS-Full Scan with internal standard SKF525A. The specimens were alkalized (pH > 10) and extracted with V(benzene):V(ethyl acetate) = 1:1, and quantitatively analyzed using GC-MS-SIM with internal standard diazepam-d5. RESULTS: The lowest detection limits of trihexyphenidyl, chlorpromazine and clozapine were 0.3, 0.3 and 0.7 ng/mL (S/N > or = 3) respectively. The calibration curve in 20-10 000 ng/mL showed a good linear distribution. The recovery rate was 79.9% to 85.5%. The RSDs of intraday and interday were less than 5.1%. CONCLUSION: The established method was simple, sensitive and accurate for simultaneous determination of trihexyphenidyl, chlorpromazine and clozapine in human blood, and can be applied in forensic toxicological cases.
Assuntos
Antipsicóticos/sangue , Clorpromazina/sangue , Clozapina/sangue , Cromatografia Gasosa-Espectrometria de Massas/métodos , Triexifenidil/sangue , Adulto , Antipsicóticos/intoxicação , Feminino , Toxicologia Forense , Humanos , Concentração de Íons de Hidrogênio , Masculino , Pessoa de Meia-Idade , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Solventes/químicaRESUMO
OBJECTIVE: To develop a specific CZE method for the determination of methamphetamine in whole blood after solid phase extraction. METHODS: With the doxapram as internal standard, Oasis column was used to extract drugs from whole blood and the sample was analysized by CZE. RESULTS: The method showed excellent linearity and the linear correlation coefficient was 0.994. The relative standard deviation for between-day and within-day were 5.31% and 2.22%, respectively. CONCLUSION: The method is effective, simple, reliable and has been used in the determination of methamphetamine in whole blood.