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Determination of a novel nonfluorinated quinolone, nemonoxacin, in human feces and its glucuronide conjugate in human urine and feces by high‐performance liquid chromatography–triple quadrupole mass spectrometry
Author(s) -
He Gaoli,
Guo Beining,
Yu Jicheng,
Zhang Jing,
Wu Xiaojie,
Cao Guoying,
Shi Yaoguo,
Tsai Chengyuan
Publication year - 2015
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.3350
Subject(s) - chemistry , chromatography , high performance liquid chromatography , glucuronide , metabolite , liquid chromatography–mass spectrometry , human feces , solid phase extraction , mass spectrometry , feces , biochemistry , paleontology , biology
Three methods were developed and validated for determination of nemonoxacin in human feces and its major metabolite, nemonoxacin acyl‐ β ‐ d ‐glucuronide, in human urine and feces. Nemonoxacin was extracted by liquid–liquid extraction in feces homogenate samples and nemonoxacin acyl‐ β ‐ d ‐glucuronide by a solid‐phase extraction procedure for pretreatment of both urine and feces homogenate sample. Separation was performed on a C 18 reversed‐phase column under isocratic elution with the mobile phase consisting of acetonitrile and 0.1% formic acid. Both analytes were determined by liquid chromatography–tandem mass spectrometry with positive electrospray ionization in selected reaction monitoring mode and gatifloxacin as the internal standard. The lower limit of quantitation (LLOQ) of nemonoxacin in feces was 0.12 µg/g and the calibration curve was linear in the concentration range of 0.12–48.00 µg/g. The LLOQ of the metabolite was 0.0010 µg/mL and 0.03 µg/g in urine and feces matrices, while the linear range was 0.0010–0.2000 µg/mL and 0.03–3.00 µg/g, respectively. Validation included selectivity, accuracy, precision, linearity, recovery, matrix effect, carryover, dilution integrity and stability, indicating that the methods can quantify the corresponding analytes with excellent reliability. The validated methods were successfully applied to an absolute bioavailability clinical study of nemonoxacin malate capsule. Copyright © 2014 John Wiley & Sons, Ltd.