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  • Determination of buprenorphine, fentanyl and LSD in whole blood by UPLC-MS-MS.

Determination of buprenorphine, fentanyl and LSD in whole blood by UPLC-MS-MS.

Journal of analytical toxicology (2013-02-21)
Thomas Berg, Benedicte Jørgenrud, Dag Helge Strand
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.

MATERIALS
Product Number
Brand
Product Description

Supelco
LSD solution, 25 μg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®
Supelco
LSD solution, 1.0 mg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®
Supelco
Calcium formate, Standard for quantitative NMR, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Cesium formate, 98%
Supelco
tert-Butyl methyl ether, analytical standard
Sigma-Aldrich
Calcium formate, BioUltra, ≥99.0% (T)
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Thallium(I) formate, 97%
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Sigma-Aldrich
Lysergic acid diethylamide
Sigma-Aldrich
tert-Butyl methyl ether, suitable for HPLC, ≥99.8%
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
tert-Butyl methyl ether, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
Sigma-Aldrich
tert-Butyl methyl ether, ACS reagent, ≥99.0%
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
tert-Butyl methyl ether, reagent grade, ≥98%
Sigma-Aldrich
tert-Butyl methyl ether, reagent grade, 98%
Sigma-Aldrich
tert-Butyl methyl ether, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Sodium formate, reagent grade, 97%
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Sodium formate, ACS reagent, ≥99.0%
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Sodium formate-13C, 99 atom % 13C
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Sigma-Aldrich
Potassium formate, ReagentPlus®, 99%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG