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Development of a Rapid and Simultaneous Detection Method for Buprenorphine, Norbuprenorphine and Naloxone in Human Plasma Using Ultra‐high Performance Liquid Chromatography‐tandem Mass Spectrometer with Solid‐phase Extraction
Author(s) -
Guo Qiaozhen,
Du Zhenxia
Publication year - 2011
Publication title -
chinese journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.28
H-Index - 41
eISSN - 1614-7065
pISSN - 1001-604X
DOI - 10.1002/cjoc.201180334
Subject(s) - chemistry , chromatography , detection limit , buprenorphine , solid phase extraction , selected reaction monitoring , mass spectrometry , extraction (chemistry) , electrospray ionization , formic acid , tandem mass spectrometry , opioid , biochemistry , receptor
A simultaneous method was successfully established and validated for the separation and determination of buprenorphine (BP), its primary metabolite, nor‐buprenorphine (NBP) and a proposed co‐formulate, naloxone (NLX) in human plasma. The method used buprenorphine‐d 4 (BP‐D 4 ), nor‐buprenorphine‐d 3 (NBP‐D 3 ), naltrexone (NTX) as internal standards (ISs). 100 μL of plasma sample fortified with the ISs was cleaned up by solid‐phase extraction (SPE), and was then separated on a Waters Acquity TM BEH C 18 column with gradient elution using methanol and water (containing 0.2% formic) at a flow rate of 0.25 mL·min −1 . The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring (MRM) mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1–25, 0.25–25 and 0.05–25 ng·mL −1 for BP, NBP and NLX, respectively, with r ≧0.9935. The method had high sensitivity (the limits of detection were 0.02, 0.1 and 0.01 ng·mL −1 for BP, NBP and NLX, respectively) and high recoveries (≧97.6%). The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bioanalytical method: intra and inter assay precisions within the required limits of ≦25% RSD. The LOQs fulfilled the LOQ requirements: precision≦25% RSD, and was fully validated according to the State Food and Drug Administration (SFDA) regulations. The results demonstrated that ultra‐high performance liquid chromatography‐tandem mass spectrometer (UPLC‐MS/MS) with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.