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Merck

LC/MS/MS Analysis of Interacting Cardiac Drugs Digoxin, Quinidine, Amiodarone and Verapamil on Titan C18

LC/MS/MS Analysis of Interacting Cardiac Drugs Digoxin, Quinidine, Amiodarone and Verapamil on Titan C18 application for LC-MS

Materials

SPE ํŠœ๋ธŒ ๋˜๋Š” ํ”Œ๋ ˆ์ดํŠธ

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HybridSPEยฎ-PLus 96-Well Plate

volume 2 mL, pk of 1 ea

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Digoxin

analytical standard

Quinidine

anhydrous

Amiodarone hydrochloride

Pharmaceutical Secondary Standard; Certified Reference Material

Verapamil hydrochloride

United States Pharmacopeia (USP) Reference Standard

CONDITIONS

sample/matrix

Sample spiked into rat plasma

SPE well plate

HybridSPEยฎ-PLus 96-Well Plate (575659-U)

condition

100 uL of spiked rat plasma was added to the HybridSPE plate well, followed by 300 uL of protein precipitation solvent, acetonitrile with 1% formic acid. (The plate, sealed, secured on a vibrater, agitated by vibration at 1000 rpm for 2 min. The plate was transfered to a vacuum manifold. Vacuum was applied at 10 in Hg for 4 min.)

column

Titan C18, 5 cm x 2.1 mm I.D., 1.9 μm particles (577122-U)

mobile phase

[A] Water; [B] methanol, both with 0.1% formic acid/10 mM ammonium formate

gradient

0-1 min, 45%B; 1.5-4 min 90%B, 4.5-8 min 45%B 

flow rate

0.2 mL/min

pressure

2900 psi

column temp.

35 ยฐC

detector

MS, ESI(+), MRM mode

injection

1 μL

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Sample pretreatment: Sample spiked into rat plasma

Detector:
MRM transitions:
Peak MRM
1. Quinidine325.2/81.1, 307.1
2. Verapamil455.3/165.1
3. Digoxin798.5/651.5
4. Amiodarone646.1/58.1, 100.1

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