LC/MS/MS Analysis of Immunosuppressant Drugs in Human Plasma on Ascentis® Express F5 after SPE Using HybridSPE®-Phospholipid

LC/MS/MS Analysis of Immunosuppressant Drugs in Human Plasma on Ascentis® Express F5 after SPE Using HybridSPE®-Phospholipid

Conditions

sample preparation SPE (Solid Phase Extraction)
SPE tube/cartridge HybridSPE-PLus 96-Well Plate, 50 mg/2 mL per well (575659-U)
sample addition 300 µl of 1% formic acid acetonitile, 100 µl spiked plasma per well
elution apply vacuum at 10 in Hg for 4 min
column Ascentis Express F5, 10 cm x 2.1 mm, I.D., 2.7 µm particles (50863-U)
column temp. 75 C
mobile phase [A] water; [B] acetonitrile:water (90:10), each with 10 mM ammonium formate
gradient 50% B for 0.5 min; to 80% B in 2 min; hold for 1.5 min; to 50% in 0.1 min; hold for 3 min
flow rate 0.3 ml/min
pressure 1300 psi (90 bar)
injection 2 µl
detector MS, ESI(+), MRM mode

Description

Analysis Note This work developed a reproducible LC/MS/MS and sample preparation method for determination of immunosuppressant drugs ascomycin, cyclosporin A, cyclosporin D, sirolimus and tacrolimus, in human plasma. HybridSPE®-PLus plates provided phospholipid-free plasma samples. UHPLC separation used an Ascentis Express F5 column. LC/MS grade solvents were used to supply low background interference and low particulate contaminants for robust, trouble-free operation. Cerilliant CRMs provided reliable identification and quantification.
Categories Analytical Chromatography, Vitamins and Natural products
Featured Industry Clinical
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC, HybridSPE is a registered trademark of Sigma-Aldrich Co. LLC
suitability application for SPE, application for HPLC

Materials

     
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