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An HPLC method for the determination of moxifloxacin in breast milk by fluorimetric detection with precolumn derivatization

Tekkeli S. E., Gazioglu I., Kiziltas M. V.

Acta Chromatographica

2017

Vol. 29, no. 1

57--65

A new, sensitive, and selective high-performance liquid chromatography (HPLC) method with fluorimetric detection was developed for the determination of moxifloxacin (MOX) in human breast milk. MOX was precolumn derivatized with fluorescamine; the fluorescent derivative was separated on an RP C18 column using a mobile phase composed of acetonitrile–10 mM orthophosphoric acid by isocratic elution with flow rate of 0.5 mL min -1. The method was based on the measurement of the derivative using fluorescence detection at 481 nm with excitation at 351 nm. The calibration curve was linear over the range of 1–40 μg Ml -1. Limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.3 and 1 μg Ml -1, respectively. Intra-day and interday repeatabilities were less than 3.15%.

Determination of cembrenediols in tobacco by gas chromatography—mass spectrometry-selected ion monitoring with precolumn derivatization

Zhou Y., Yang Y., Li X. L., Chen Z. Y., Liu Q. B., Zhu X. L., Yang J.

Acta Chromatographica

2016

Vol. 28, no. 4

513--524

An efficient and sensitive analytical method based on precolumn derivatization and gas chromatography—mass spectrometry—selected ion monitoring (GC—MS—SIM) was proposed and validated for analysis of two cembrenediols (CBDs) which are α-cembrenediol and β-cembrenediol in tobacco samples. CBDs in tobacco samples were extracted by sonication with 50 mL dichloromethane for 10 min before derivatized with 2:3 (v/v) bis(trimethylsilyl)trifluoroacetamide (BSTFA)—pyridine at 20 °C for 100 min. CBDs’ level in tobacco samples was analyzed by GC—MS—SIM and quantified by the internal standard method. The linear range for α-CBD and β-CBD was 13.6–554.6 μg Ml-1 and 4.11–162.6 μg Ml-1, and the correlation coefficients of both were 0.9998. The limit of detection (LOD) and limit of quantification (LOQ) of α-cembrenediol and β-cembrenediol were 0.40 μg g−1 and 1.34 μg g-1, and 0.27 μg g−1 and 0.90 μg g−1, respectively. Average recoveries of α-CBD and β-CBD were 94.4–99.9% and 91.9–98.2% while the relative standard deviations (RSDs, n = 5) were ranged from 2.67 to 5.6% and 2.04 to 4.22%, respectively. This proposed analytical method has been successfully applied to analyze CBDs in tobacco samples.