Validation of a chromatographic method for amoxicillin determination in wastewaters after its degradation by advanced oxidation process

Abstract

A rapid analytical procedure based on high performance liquid chromatography for identification and quantification of amoxicillin in wastewaters after its degradation by advanced oxidation process (AOP) was developed and validated. The proposed methodology was validated concerning to linearity, precision, limit of quantification, and limit of detection according to the required INMETRO and ANVISA (regulatory agencies in Brazil) standards. The method was applied to the determination of amoxicillin in wastewaters from wastewater treatment plant of a Brazilian pharmaceutical industry spiked with amoxicillin after AOP treatment process on a pilot scale reactor. The method allows the determination of the referred drug in a concentration range of 10-100 mg L −1 with a detection limit of 2.32 mg L −1 , a quantification limit of 7.04 mg L −1 , and enabling control of contaminant removal.

A Validated HPLC Multichannel DAD Method for the Simultaneous Determination of Amoxicillin and Doxycycline in Pharmaceutical Formulations and Wastewater Samples

“…The different matrices used to prepare the calibration curves were analyzed previously with the HPLC-DAD method, and no Amox and Dox levels were detected. High values of the correlation coefficients (R 2 = 0.9999) were also obtained for the determination of Amox in tablets [6,41] and water [42], and for Dox in tablets [33] and water [44] by HPLC.…”

“…Therefore, an interm length should have been chosen for an even response from bought compound run on a single wavelength, resulting in a method with lower chromatograp ters, and a higher limit of detection (LOD) and limit of quantification (L quently, two different wavelengths (230 and 350 nm) were selected to monit tention time at 1.70 min) and Dox (retention time at 5.23 min) (Figure 2). The proposed method for the simultaneous determination of Amox and maceutical formulations and wastewater samples was validated relating to th of the chromatographic parameters (tailing factor, resolution, peak symmetr plates), LOD, LOQ, working and linear ranges, precision, and recovery, acco The proposed method for the simultaneous determination of Amox and Dox in pharmaceutical formulations and wastewater samples was validated relating to the conformity of the chromatographic parameters (tailing factor, resolution, peak symmetry, theoretical plates), LOD, LOQ, working and linear ranges, precision, and recovery, according to current guidelines and previously published papers [41][42][43][44][45][46][47].…”

“…Preferably, the calibration range should be set so that most analyte concentrations fall near the range's center. Since we intended to develop and validate an analytical method to quantify the amoxicillin and doxycycline in various matrices (wastewater, tab), based on the previous studies [6,[41][42][43][44], we established an optimal, large range of calibration from the LOQ to 100 ug/mL to be relevant for each investigated matrix. Moreover, the calibration curves were forced to go through the origin resulting in high accuracy at low concentrations, which is proven by the repeatability of the LOQ (Table 2).…”