Determination of Buprenorphine, Fentanyl and LSD in Whole Blood by UPLC-MS-MS

Abstract

A sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method has been developed and validated for the quantification of buprenorphine, fentanyl and lysergic acid diethylamide (LSD) in whole blood. Sample preparation was performed by liquid-liquid extraction (LLE) with methyl tert-butyl ether. UPLC-MS-MS analysis was performed with a mobile phase consisting of ammonium formate (pH 10.2) and methanol. Positive electrospray ionization MS-MS detection was performed with two multiple reaction monitoring transitions for each of the analytes and the deuterium labeled internal standards. Limit of detection values of buprenorphine, fentanyl and LSD were 0.28, 0.044 and 0.0097 ng/mL and limit of quantification values were 0.94, 0.14 and 0.036 ng/mL, respectively. Most phospholipids were removed during LLE. No or only minor matrix effects were observed. The method has been routinely used at the Norwegian Institute of Public Health since September 2011 for qualitative and quantitative detections of buprenorphine, fentanyl and/or LSD in more than 400 whole blood samples with two replicates per sample.

Determination of a selection of synthetic cannabinoids and metabolites in urine by UHPSFC‐MS/MS and by UHPLC‐MS/MS

“…We tested both the Acquity UPC 2 BEH 2‐EP and the Acquity UPC 2 BEH with the basic mobile phase, and the best peak shapes were obtained with the UPC 2 BEH column (data not shown). UHPLC‐MS/MS analysis was performed with the similar mobile phase composition, the same gradient profile, and the same column, used in other methods for drug detections in our laboratory . For the aqueous part of the mobile phase, 5 mM ammonium formate with pH 10.2 was used, instead of 5 mM ammonium bicarbonate with pH 10.2, since the latter, according to Amundsen et al ., pollutes the ESI source.…”

“…The flow rate was 0.4 mL/min, and the injection volume was 0.2 μL. The gradient profile was similar to one used in a previous publication [37] : 5% B in 0.00-0.15 min, 5-30% B in 0.15-0.30 min, 30-50% B in 0.30-2.70 min, 50-90% B in 2.70-3.80 min, 90% B in 3.80-4.20 min, 90-98% B in 4.20-4.30 min, 98% B in 4.30-6.00 min, 98-5% B in 6.00-6.10 min, and 5% B in 6.10-6.80 min. The total cycle time, from injection to injection, was 7.5 min, but all compounds were eluted within 4.5 min.…”

Use of high‐pH (basic/alkaline) mobile phases for LC–MS or LC–MS/MS bioanalysis

“…Once chromatographers experience the benefits of high‐pH mobile phases, they will not limit themselves just to acidic mobile phases anymore. Whenever a situation calls for it, they will not hesitate to use high‐pH mobile phases (Berg, Lundanes, Christophersen, & Strang, ; Berg, Jørgenrud, & Strand, ; Heinig et al, ; Heinig et al, ; Tan et al, ; Tan et al, ; Verplaetse and Tytgat, & ; Verplaetse, Cuypers, & Tytgat, ).…”

Drugged driving arrests in Norway before and after the implementation of per se law

“…High-performance liquid chromatography with tandem mass spectroscopy (LC-MS/MS) was used for analysing a selection of illicit drugs, sedatives, hypnotics and analgesics [20]. The confirmation analyses of tetrahydrocannabinol (THC) were done by GC-MS [21], for amphetamine and methamphetamine by GC-MS [22], for benzodiazepines by LC-MS/MS [23], for heroin and the metabolites by LC-MS/MS [24], for other opiates by UHPLC-MS/ MS [25], for GHB by UHPLC-MS/MS [26], for LSD by UHPLC-MS/SM [27] and for z-hypnotics by LC-MS in 2010-2011 [28] and by UHPLC-MS/MS during 2012-2013 using liquid-liquid extraction, separation on a 10 cm C18 column with 1.7 mm particle size and alkaline mobile phase (E. Eliassen and L. Kristoffersen, manuscript submitted for publication).…”