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2 2021

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Optimization and validation of Eco-friendly RP-HPLC and univariate spectrophotometric methods for the simultaneous determination of Fluorometholone and Tetrahydrozoline hydrochloride

Essam Hebatallah M., Saad Martin N., Elzanfaly Eman S., Amer Sawsan M.

Acta Chromatographica

2021

Vol. 33, no. 3

216--227

A sensitive RP-HPLC method is presented for the simultaneous quantification of Fluorometholone (FLM) and Tetrahydrozoline hydrochloride (THZ). The method has the advantages of being rapid, accurate, reproducible, ecologically acceptable and sensitive. The separation utilized C8 Xbridge® column and mobile phase mixture of Acetonitrile/phosphate buffer pH 3 ± 0.1 (70:30, v/v) with UV detection at 230 nm. Stepwise optimization and factors affecting separation are properly discussed. Different factors were optimized such as stationary phase, selection of organic solvent and its content, buffer pH and concentration, flow rate, elution type and detection wavelength. The studied drugs were efficiently separated in 3.4 min with high resolution. Also, two univariate spectrophotometric methods have been optimized for the quantification of the studied drugs. Method 1: dual wavelength for THZ and iso-absorptive point for FLM, Method 2: ratio difference (RD) for THZ and first derivative FLM utilizing methanol as a solvent. These methods are accurate, precise with minimal data manipulation. Greenness of the methods was estimated using eco-scale tool where the presented methods were found to be excellent green with eco-score of 83 for HPLC and 80 for spectrophotometry. The methods are validated in conformance with ICH guidelines, with acceptable accuracy, precision, and selectivity. The suggested methods can be employed for the economic analysis of THZ and FLM in their pure form and binary ophthalmic formulation, that can be employed by quality control laboratories.

Analytical quality by design approach for the control of potentially counterfeit chloroquine with some NSAIDS using HPLC with fluorescence detection in pharmaceutical preparation and breast milk

Hassan Said A., Ibrahim Noha, Elzanfaly Eman S., El Gendy Ahmed E.

Acta Chromatographica

2021

Vol. 33, no. 3

234--244

Chloroquine phosphate (CQ) the antimalarial drug and suggested to treat the pandemic disease coronavirus (COVID-19) is often adulterated with some of the non-steroidal anti-inflammatory drugs (NSAIDs) such as paracetamol, aspirin (ASP), or both. The purpose of this study is to detect such counterfeited drugs, using a reversed phase high pressure liquid chromatography (RP-HPLC) method with fluorescence detection. Analysis was divided into three phases. In the first phase, a Plackett-Burman design (PBD) was used to screen five independent factors, namely, buffer pH, buffer concentration (mM), acetonitrile content (%), flow rate (mL/min) and triethylamine (TEA) content in the buffer preparation (%). The selected dependent variables were (resolution, symmetry of peaks and run time). The objective of the second phase was to optimize the method performance using Box-Behnken design (BBD) and desirability function for multiple response optimization to obtain the best chromatographic performance with the shortest run time. Optimal chromatographic separation was achieved on a YMC-pack pro C18 ODS-A column (15 cm × 4.6 mm, 5 µm) at room temperature The optimum mobile phase consisted of acetonitrile and 5 mM sodium dihydrogen phosphate buffer containing 0.5% triethyamine (30:70, v/v) with the pH adjusted to 3.5 using an orthophosphoric acid solution. The flow rate was maintained at 1 mL/min, and the detection was performed with a fluorescence detector fixed at 380 nm(λemission) after excitation at 335 nm(λexcitation). The third phase was method validation according to ICH guidelines, providing to be specific, precise, accurate, and robust. The method is linear over a range of 0.4–8 µg/mL for chloroquine and ASP, while for paracetamol it is linear over 16–48 µg/mL. The developed RP-HPLC method was used for quantitation of the three drugs in chloroquine dosage form samples. The method shows a great tendency in the classification between the genuine chloroquine and the adulterated ones in pharmaceutical preparations and breast milk.