High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine

Abstract

A highly specific, sensitive, and rapid method, to quantify gemifloxacin in human urine using HPLC coupled to the triple quadrupole mass spectrometer system, was developed and validated. Gemifloxacin and ofloxacin (internal standard) were rapidly extracted from urine samples without any tedious pretreatment procedure. Urine samples were filtered through a Millex-GP, 0.22 m syringe filter. Optimal chromatographic separation of the analytes was achieved on Zorbax SB-C 18 (30 mm × 2 mm i.d., 3.5 m maintained at ambient temperature). The mobile phase consisted of 0.1% formic acid (pH 3.2) and acetonitrile (80 : 20) and a flow rate of 0.2 mL min −1 for 4 min. The analytes were monitored by electrospray ionization in positive ion multiple reaction monitoring mode. The method provided a linear response ( = 0.9998) from a quantitation range of 5 ng mL −1 to at least 500 ng mL −1 . The mean extraction recovery % of gemifloxacin from spiked human urine was 101.33 ± 2.58%. The reproducibility of the method was reliable with the intra-and inter-day precision of <2% and accuracy within 2%. The established method was reliably applied for the determination of gemifloxacin in volunteers' urine samples with the mean recoveries of gemifloxacin from Factive tablets 320 mg > 97.0%.

Validated liquid chromatography tandem mass spectrometry for simultaneous quantification of foretinib and lapatinib, and application to metabolic stability investigation

“…Validation parameters of the established LC-MS/MS method were described in more detail previously 15,18,19 that included assay recovery, sensitivity, specicity, linearity, reproducibility, limit of detection (LOD) and limit of quantication (LOQ). The least squares statistical method was used to calculate the calibration curve equations (y ¼ ax + b).…”

Reactive intermediates in copanlisib metabolism identified by LC-MS/MS: phase I metabolic profiling

“…Aliquots of 10 mL of each reconstituted sample were analyzed using LC-MS/MS system. [30][31][32] Replicates of blank sample were analyzed at the same run to conrm the absence of the proposed metabolites or adducts (ESI Fig. S11-S20 †).…”

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“…It is widely used for treatment of respiratory infections (bronchitis, pneumonia) and urinary infections. A few analytical techniques have been constructed for the quantification of Gemifloxacin in pure forms, such as, Spectrophotometric method [25][26] , HPTLC 27 , RP-HPLC [28][29] , LC-MS 30 , UV-Spectrofluorometric method 31 and Zone electrophoresis 32 .…”