Eco-Friendly Green Liquid Chromatographic for Determination of Doxycycline in Tablets and in the Presence of Its Degradation Products

Abstract

Doxycycline, an oral antimicrobial, does not present a sustainable analytical method described in the literature using liquid chromatography. A new and efficient method was developed and validated for the quantification of doxycycline tablets by HPLC-UV. Its aim is the contribution to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. The HPLC-UV method used a mixture of purified water + 0.5 % acetic acid and ethanol (40:60, v/v). The flow rate was 0.8 mL min-1, C18 Luna column, 20 μL of injected volumes at 275 nm. The samples were prepared in purified water and the method was linear over the concentration range of 20–200 μg mL-1 (r = 0.9997) with limits of detection and quantification of 1.08 and 3.27 μg mL-1, respectively. The precision of the method showed RSD 0.50 % (intra-assay), 2.35 % (inter-assay) and 1.13 % (between analysts). The accuracy of the method was determined by standard recovery and it was 99.85 %. The DOX tablets were subjected to oxidative, acid, basic, neutral and photolytic degradation and it showed be stability indicative. Statistical analysis provided reliable, safety and reproducible results. The method is considered linear, selective, precise, accurate, robust, indicative of stability and safe to be used in routine quality control analyzes for determination and quantification of doxycycline in tablets. The proposed method is an ecologically correct alternative for the evaluation of doxycycline tablets.

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

“…The LOQs of the optimized method were low enough to perform the quantitative determination of Amox and Dox in a variety of matrices. Our study's LOD and LOQ values are much lower than those of 0.436 and 1.32 µg/mL [20], 2.14 and 7.15 µg/mL [54], 1.579 and µg/mL, 0.1 and 0.3 mg/mL [41], and 4.785 µg/mL [17] reported for the quantitative determination of Amox, and 1.08 and 3.27 µg/mL [55], and 16 and 54 µg/L [6] stated for Dox in pharmaceutical formulations and wastewater samples using the HPLC method.…”

Determination of Doxycycline as Pure and in Pharmaceutical Preparation (Capsule) Using 4-Aminoantipyrine in Presence of Potassium Periodate

“…Various analytical methods have been reported in literature included estimation of Doxycycline in pure and dosage forms, including highperformance liquid chromatography (NP-HPLC and RP-HPLC) (Ghidini et al, 2018;Mileva, 2019;Mashru and Koshti, 2021;Dil et al, 2020), HPLC-mass (Permana et al, 2019), HPTLC (Kumssa et al, 2021), potentiometric sensor (Ali et al, 2018), ratiometric probe (Tian and Fan, 2021), flow injection spectrophotometry (Tawfeeq and Qassim, 2020), Fluorometric (Sun, 2018) and the spectrophotometry methods using various reagents: Fe(II) with 1,10-phenanthroline (method A) and Fe (II) with 2,2'-bipyridyl (method B) (Awad and Taki, 2021), 4-aminoantipyren in presence of potassium ferriecyanide in alkaline medium. (Al-Kalissy and Mohammed, 2015) diazotized benzocaine (Abbas et al, 2020) and UV-spectrometric method at 260 nm (Patil et al, 2020), simultaneous estimation of doxycycline and levofloxacin using wavelengths 273 nm and 287nm in measurements respectively, and iso-absorptive point at 280 nm in phosphate buffer pH 6.8 prepared in Water: Methanol (80:20) (Gholse et al, 2022), Some of the previous methods required heating, and some of them needs expensive apparatus, therefore we developed spectrophotometric method for the estimation of doxycycline as pure and in its dosage form, based on oxidative coupling reaction using 4-aminoantipyrene as a reagent and in the presence of potassium periodate.…”