A sensitive and robust lc-ms/ms method with monolithic column and electrospray ionization for the quantitation of efavirenz in human plasma: application to a bioequivalence study

Abstract

Recebido em 12/7/10; aceito em 17/12/10; publicado na web em 25/3/11An LC-MS/MS method has been developed for the determination of efavirenz (EFZ) in human plasma using hydrochlorothiazide as internal standard (I.S.). An ESI negative mode with multiple reaction-monitoring was used monitoring the transitions m/z 313.88→69.24 (EFZ) and 296.02→204.76 (I.S.). Samples were extracted using liquid-liquid extraction. The total run time was 2.0 min. The separation was achieved with HPLC-RP using a monolithic column. The assay was linear in the concentration range of 100 -5000 ng mL -1 . The mean recovery was 83%. Intra-and inter-day precision were < 9.5% and < 8.9%, respectively and accuracy was in the range ± 8.33%. The method was successfully applied to a bioequivalence study.

Correlation between microstructure and bioequivalence in Anti-HIV Drug Efavirenz

“…The reference drug product (Stocrin Ò , 600 mg tablets) was commercially available at the time of the study. Details of clinical data from the approved biobatch can be found in Honorio et al [10], and for the not approved biobatch in Bedor et al [9]. Prior to volunteer recruitment, all protocols were approved by the research ethics committee, as detailed in each specific study.…”

“…The bioequivalence studies were conducted on volunteers whose age ranged between 18 and 45 years. The analytical tests and details of these studies were reported by Bedor et al [9] and Honorio et al [10], who followed the Brazilian protocol for bioequivalence studies [11], in accordance also with international recommendations for this kind of evaluation. Apart from the in vivo studies, so far there are no clear explanations for the dissolution (in vitro) tests with the specific conditions used in this work.…”

Characterization, in vitro dissolution, and pharmacokinetics of different batches of efavirenz raw materials

“…The average analysis time was 8 min. The plasma concentration of EFV was determined using HPLC coupled to a mass detector (LC-MS/ MS 3200 QTRAP from Sciex V R , Toronto, Canada), following a previously described protocol [28]. An isocratic elution mode of the analytes from an Onix C18 monolithic column (L: 50 mm; i.d: 4.6 mm) (Phenomenex V R , Torrance, USA) was achieved with a mobile phase consisting of acetonitrile/water (50:50 v/v þ 5% isopropyl alcohol, v/v).…”

Разработка Методики Изолирования Эфавиренза Из Мочи

“…Проведенный анализ литературы и нормативных документов по контролю качества эфавиренза [4,7,9,10] показал, что рекомендованным методом количественного определения исследуемого лекарственного средства является метод высокоэффективной жидкостной хроматографии.…”