UHPLC/MS Analysis of Drugs in Whole Blood on Titan C18 after Biocompatible Solid Phase Microextraction (BioSPME) using SPME LC Tips with C18 Chemistry
Materials
SPME fiber
standard
Carbamazepine solution
1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®Diazepam solution
1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®Metoprolol tartrate solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Propranolol hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®CONDITIONS
sample preparation
Solid Phase Microextraction
sample/matrix
whole blood spiked at 10 ng/mL
SPME fiber
SPME LC Tips (57234-U)
extraction
whole blood, 15 minutes
desorption process
methanol 30 minutes
column
Titan C18, 5 cm x 2.1 mm I.D., 1.9 μm particles (577122-U)
mobile phase
[A] 5 mM ammonium formate, pH 4; [B] 5 mM ammonium formate in acetonitrile:water (90:10, A:B)
gradient
30 to 70% B in 3 min
flow rate
0.3 mL/min
column temp.
35 °C
detector
MS, ESI+, MRM
sample
3 μL
Description
Analysis Note
Solid phase microextraction (SPME) is a viable technique for microsampling of biological matrices for subsequent HPLC, UHPLC, and LC/MS analysis. The fibers allow direct sampling without additional sample treatment. The concentration effect of the fibers provides increased analyte sensitivity compared to other techniques. Shown here is the separation of a set of drugs on a Titan C18 UHPLC column after using SPME LC tips to extract them from whole blood. The highest grade solvents provided clean, robust operation. Cerilliant CRMs provided reliable quantification.
Legal Information
null