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

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

Materialien

Analytische Säule

Produkt-Nr.
Beschreibung
Preisangaben

53939-U

Ascentis® Express HILIC HPLC Column

2.7 μm particle size, L × I.D. 10 cm × 2.1 mm

SPE-Röhrchen oder -Platte

Produkt-Nr.
Beschreibung
Preisangaben

575656-U

HybridSPE®-Phospholipid

96-well Plate, bed wt. 50 mg, volume 2 mL, pk of 1

Standard

Produkt-Nr.
Beschreibung
Preisangaben

F-017

(±)-Flecainide solution

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

L-018

Lidocaine solution

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

Zubehör

Produkt-Nr.
Beschreibung
Preisangaben

Z654760

IKA® VORTEX 3

vortex shaker, 115V, 1/cs

Z654779

IKA® VORTEX 3

vortex shaker, 230V, 1/pk

CONDITIONS

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

Beschreibung

Hinweis zur Analyse

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.

Rechtliche Hinweise

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

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