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A highly sensitive LC‐MS/MS method capable of simultaneously quantitating celiprolol and atenolol in human plasma for a cassette cold‐microdosing study

2011; Wiley; Volume: 34; Issue: 13 Linguagem: Inglês

10.1002/jssc.201100089

1615-9314

Yoshiyuki Minamide, Yukio Osawa, Hiroshi Nishida, Harue Igarashi, Shinobu Kudoh,

Analytical chemistry methods development

Abstract A highly sensitive simultaneous quantitative method for a cassette cold‐microdosing study on celiprolol and atenolol was developed with liquid chromatography–tandem mass spectrometry. The method utilizes a combination of solid‐phase extraction (SPE) with strong cation exchange (SCX) cartridge columns and reversed‐phase chromatography with an ODS analytical column. SCX‐SPE cartridge columns (100 mg sorbent) were used for a selective extraction of celiprolol, atenolol and metoprolol (internal standard) from 500 μL of human plasma samples. Turbo‐ion spray at positive mode was employed for the ionization of the drug compounds. Quantitation was performed on a triple quadrupole mass spectrometer by selected reaction monitoring with the transitions of m / z 380 to m / z 251 for celiprolol and m / z 267 to m / z 145 for atenolol. Separation of analytes was achieved on an ODS column (100 mm length×2.1 mm id, 3 μm) by a gradient elution with 10 mM formic acid and methanol by varying their proportion at a flow rate of 0.2 mL/min. The method was validated in the range of 1–250 pg/mL for celiprolol and 2.5–250 pg/mL for atenolol and was successfully applied to the elucidation of pharmacokinetic profiling in a cold cassette microdosing study of the β‐blockers.