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G005818

LC/MS (TOF) Analysis of Antiarrhythmic Drugs and Metabolites in Plasma on Ascentis® Express HILIC after Sample Prep using HybridSPE®-Phospholipid

application for HPLC

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About This Item

technique(s)

HPLC: suitable

test parameters

sample preparation: SPE (Solid Phase Extraction)
sample/matrix: rat plasma stabilized with K2EDTA was spiked directly from stock standard to a level of 400 ng/mL
SPE tube/cartridge: HybridSPE-Phospholipid 96-Well Plate, 50 mg/2 mL (575656-U)
sample addition: apply 100 μL of plasma to plate, followed by 300 μL of 1% formic acid acetonitrile. Agitate via vortex for 4 min
elution: place on vacuum manifold and apply 10” Hg vacuum for 4 minutes. Collect filtrate and analyze directly.
column: Ascentis Express HILIC, 10 cm x 2.1 mm I.D., 2.7 μm particles (53939-U)
mobile phase: [A] 5 mM ammonium formate; [B] 5 mM ammonium formate in acetonitrile; (5:95, A:B, pH 7.0 with formic acid)
flow rate: 0.4 mL/min
pressure: 1305 psi (90 bar)
column temp.: 35 °C
detector: ESI(+), full scan, m/z 100-1000
injection: 0.5 μL
sample: plasma extract, analyte concentration of final sample work up is equivalent to 100 ng/mL

suitability

application for HPLC

application(s)

clinical

Analysis Note

The basic characteristics of these compounds make them targets for HILIC chromatographic separation. HILIC mobile phases consist of a high composition of acetonitrile, which facilitates the direct analysis of precipitated plasma samples without the need for additional sample solvent exchange. In most cases, the high organic mobile phase also facilitates increased analyte response in ESI(+) MS detections. This application used HybridSPE-Phospholipid sample prep to remove phospholipids and precipitated proteins prior to LC/MS analysis on an Ascentis Express HILIC Fused-Core HPLC column. The highest grade solvents provided clean, robust operation. Cerilliant CRMs provided reliable quantification. The resulting method was robust and sensitive.

Legal Information

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
HybridSPE is a registered trademark of Merck KGaA, Darmstadt, Germany

Analyte

Description
    Amiodarone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®
    N-Desethylamiodarone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®
    Lidocaine solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®
    (±)-Flecainide solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

SPE tube or plate

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accessory

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analytical column

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standard

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