RESUMO
Busulfan is an alkylating agent widely used in the ablation of bone marrow cells before hematopoietic stem cell transplant. Due to large intraindividual and interindividual variations, and narrow therapeutic window, therapeutic drug monitoring of busulfan is warranted. A quick and reliable HPLC-MS/MS method was developed for the assay of plasma busulfan. HPLC involved C18 column, and MS/MS was used in electrospray ionization (ESI) positive mode. Quantitation and identification of busulfan was made using various multiple reactions monitoring (MRMs). Isotopic labeled busulfan-d8 was used as the internal standard. The method is linear from 50 to 2500 ng/mL and has with-in run and between-run imprecision of <10 %.
Assuntos
Bussulfano/sangue , Cromatografia Líquida de Alta Pressão/métodos , Imunossupressores/sangue , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão/economia , Monitoramento de Medicamentos/economia , Monitoramento de Medicamentos/métodos , Humanos , Espectrometria de Massas por Ionização por Electrospray/economia , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/economiaRESUMO
Marijuana, which is made from crushing the leaves, flowers, and sometimes the stems of the plant Cannabis sativa, contains more than 30 cannabinoids. The major psychoactive cannabinoid is delta-9-tetrahydrocannabinol (THC). The major metabolite of THC, 11-nor-delta 9-carboxy-tetrahydrocannabionol (THC-COOH), is excreted in the urine primarily as a glucuronide conjugate and is commonly analyzed in biological specimens for detecting marijuana usage. The procedure described here involves the addition of deuterated internal standard THC-COOH-d9 into the sample followed by hydrolysis of conjugated THC-COOH by alkali. THC-COOH is extracted from urine or blood using liquid-liquid extraction followed by preparation of its trimethylsilyl derivatives. The analysis of derivatized THC-COOH is performed using gas-chromatography/mass spectrometry (GC/MS). Quantification of the drug in a sample is achieved by comparing the responses of the unknown sample to the responses of the calibrators using selected ion monitoring.