A highly sensitive and cost-effective HPTLC method was developed for the determination of rivastigmine hydrogen tartarate (RIV) in bulk and capsules. Moreover, magnetic solid phase extraction procedure (MSPE) was performed for analysis of RIV in human plasma to preconcentrate RIV and decrease interference from plasma constituents. The magnetic nanoparticles (MNPs) were prepared by co-precipitation process and characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), powdered X-ray diffraction (PXRD) and dynamic light scattering (DLS). These prepared MNPs have shown high extraction efficiency and all parameters affecting the adsorption of RIV on the MNPs were fully investigated. The method was validated according to FDA bio-analytical guidelines and was found to be linear over the range of 30.2–648 ng/spot. The LLOQ and LOD were 26.2 and 8.6 ng/spot, respectively.

A highly sensitive and cost-effective HPTLC method was developed for the determination of rivastigmine hydrogen tartarate (RIV) in bulk and capsules. Moreover, magnetic solid phase extraction procedure (MSPE) was performed for analysis of RIV in human plasma to preconcentrate RIV and decrease interference from plasma constituents. The magnetic nanoparticles (MNPs) were prepared by co-precipitation process and characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), powdered X-ray diffraction (PXRD) and dynamic light scattering (DLS). These prepared MNPs have shown high extraction efficiency and all parameters affecting the adsorption of RIV on the MNPs were fully investigated. The method was validated according to FDA bio-analytical guidelines and was found to be linear over the range of 30.2–648 ng/spot. The LLOQ and LOD were 26.2 and 8.6 ng/spot, respectively.

Nowadays, drug pollution; a form of water pollution caused by some pharmaceuticals and their metabolites resulting from consumers, industry and hospitals was reported. Colchicine (CLN) is considered one of the pharmaceutical wastewater contaminants which are not eliminated completely in municipal sewage treatment plants and are discharged into receiving water. Due to the higher toxicity of CLN, a novel heterogeneous Fenton's-like catalysis was established for complete degradation of CLN. So, a highly sensitive and specific liquid chromatographic method with quadrupole mass spectrometry (LC/Q-MS) was developed and validated for estimation of CLN in its pure form and in the presence of its degradation product. Herein, GraceSmart RP C18 column was utilized for separation of the cited drug (Retention time tR = 5.578 min) using methanol: water (55: 45, v/v) at 1.0 mL min−1. Detection was performed by Agilent 6120 Quadrupole MS detector in a positive ionization mode. Thereafter and for the first time, degradation of CLN by heterogeneous Fenton's-like catalysis using modified polyacrylonitrile (PAN) as a catalyst with H2O2 in aqueous acidic medium was performed. This process was firstly optimized by HPLC/UV detection at 248 nm using the aforementioned chromatographic conditions. As a result, CLN degraded completely within 30 min. The only observed degradation product was the biologically active, potent and less toxic antitumor metabolite of CLN (3- demethyl CLN) which was collected, extracted, and analyzed by Fourier Transfer- Infrared Spectroscopy (FTIR) and 13Carbon- Nuclear Magnetic Resonance (13C NMR). Finally, this method is eco-friendly and complies with the requirements of the green chemistry. It is suitable for complete removal of CLN and/or its metabolite contaminants from wastewater samples and estimation of the target drug without any interference from its degradation products. However, further study is required to expand the method applicability to the pharmaceutical wastewater treatment as well the production of 3- demethyl CLN on a large scale.

Nowadays, drug pollution; a form of water pollution caused by some pharmaceuticals and their metabolites resulting from consumers, industry and hospitals was reported. Colchicine (CLN) is considered one of the pharmaceutical wastewater contaminants which are not eliminated completely in municipal sewage treatment plants and are discharged into receiving water. Due to the higher toxicity of CLN, a novel heterogeneous Fenton's-like catalysis was established for complete degradation of CLN. So, a highly sensitive and specific liquid chromatographic method with quadrupole mass spectrometry (LC/Q-MS) was developed and validated for estimation of CLN in its pure form and in the presence of its degradation product. Herein, GraceSmart RP C18 column was utilized for separation of the cited drug (Retention time tR = 5.578 min) using methanol: water (55: 45, v/v) at 1.0 mL min−1. Detection was performed by Agilent 6120 Quadrupole MS detector in a positive ionization mode. Thereafter and for the first time, degradation of CLN by heterogeneous Fenton's-like catalysis using modified polyacrylonitrile (PAN) as a catalyst with H2O2 in aqueous acidic medium was performed. This process was firstly optimized by HPLC/UV detection at 248 nm using the aforementioned chromatographic conditions. As a result, CLN degraded completely within 30 min. The only observed degradation product was the biologically active, potent and less toxic antitumor metabolite of CLN (3- demethyl CLN) which was collected, extracted, and analyzed by Fourier Transfer- Infrared Spectroscopy (FTIR) and 13Carbon- Nuclear Magnetic Resonance (13C NMR). Finally, this method is eco-friendly and complies with the requirements of the green chemistry. It is suitable for complete removal of CLN and/or its metabolite contaminants from wastewater samples and estimation of the target drug without any interference from its degradation products. However, further study is required to expand the method applicability to the pharmaceutical wastewater treatment as well the production of 3- demethyl CLN on a large scale.

Nowadays, drug pollution; a form of water pollution caused by some pharmaceuticals and their metabolites resulting from consumers, industry and hospitals was reported. Colchicine (CLN) is considered one of the pharmaceutical wastewater contaminants which are not eliminated completely in municipal sewage treatment plants and are discharged into receiving water. Due to the higher toxicity of CLN, a novel heterogeneous Fenton's-like catalysis was established for complete degradation of CLN. So, a highly sensitive and specific liquid chromatographic method with quadrupole mass spectrometry (LC/Q-MS) was developed and validated for estimation of CLN in its pure form and in the presence of its degradation product. Herein, GraceSmart RP C18 column was utilized for separation of the cited drug (Retention time tR = 5.578 min) using methanol: water (55: 45, v/v) at 1.0 mL min−1. Detection was performed by Agilent 6120 Quadrupole MS detector in a positive ionization mode. Thereafter and for the first time, degradation of CLN by heterogeneous Fenton's-like catalysis using modified polyacrylonitrile (PAN) as a catalyst with H2O2 in aqueous acidic medium was performed. This process was firstly optimized by HPLC/UV detection at 248 nm using the aforementioned chromatographic conditions. As a result, CLN degraded completely within 30 min. The only observed degradation product was the biologically active, potent and less toxic antitumor metabolite of CLN (3- demethyl CLN) which was collected, extracted, and analyzed by Fourier Transfer- Infrared Spectroscopy (FTIR) and 13Carbon- Nuclear Magnetic Resonance (13C NMR). Finally, this method is eco-friendly and complies with the requirements of the green chemistry. It is suitable for complete removal of CLN and/or its metabolite contaminants from wastewater samples and estimation of the target drug without any interference from its degradation products. However, further study is required to expand the method applicability to the pharmaceutical wastewater treatment as well the production of 3- demethyl CLN on a large scale.

An innovative, simple, fast, specific and sensitive high performance liquid chromatographic method with ultraviolet detection (HPLC/UV) was established and validated for simultaneous determination of a combination of three commonly prescribed antigout drugs namely; Colchicine (CLN), Probenecid (PRD) and Febuxostat (FBX) in dosage forms and in human urine samples. GraceSmart RP C18 column was utilized for separation of the studied mixture using isocratic mode of mobile system consisting of acetonitrile: water (55: 45, v/v; containing 0.5% v/v formic acid). Flow rate and detection wavelengths programming were designed to obtain a rapid and efficient separation. The cited drugs were separated within 9 min. The retention times (tR) were 3.597, 5.357 and 8.250 for CLN, PRD and FBX; respectively. The linearity range for all the investigated drugs was 0.040–50.0 μg/mL with detection limits of 1.94–6.48 ng/mL. Additionally, the developed method was validated according to ICH and US-FDA guidelines and was successfully applied for simultaneous estimation of the studied drugs in their pure form, and in laboratory-made mixture solution of their respective tablets. The proposed method was also used for analysis of CLN and PRD in their combined tablets and in human urine samples obtained from healthy volunteers with good recoveries (98.39–101.87%). Furthermore, the stability of CLN-PRD mixture in urine samples was studied. In conclusion, this method is suitable for quality control purposes for simultaneous analysis of these co-administered antigout drugs in their binary and ternary mixtures.

An innovative, simple, fast, specific and sensitive high performance liquid chromatographic method with ultraviolet detection (HPLC/UV) was established and validated for simultaneous determination of a combination of three commonly prescribed antigout drugs namely; Colchicine (CLN), Probenecid (PRD) and Febuxostat (FBX) in dosage forms and in human urine samples. GraceSmart RP C18 column was utilized for separation of the studied mixture using isocratic mode of mobile system consisting of acetonitrile: water (55: 45, v/v; containing 0.5% v/v formic acid). Flow rate and detection wavelengths programming were designed to obtain a rapid and efficient separation. The cited drugs were separated within 9 min. The retention times (tR) were 3.597, 5.357 and 8.250 for CLN, PRD and FBX; respectively. The linearity range for all the investigated drugs was 0.040–50.0 μg/mL with detection limits of 1.94–6.48 ng/mL. Additionally, the developed method was validated according to ICH and US-FDA guidelines and was successfully applied for simultaneous estimation of the studied drugs in their pure form, and in laboratory-made mixture solution of their respective tablets. The proposed method was also used for analysis of CLN and PRD in their combined tablets and in human urine samples obtained from healthy volunteers with good recoveries (98.39–101.87%). Furthermore, the stability of CLN-PRD mixture in urine samples was studied. In conclusion, this method is suitable for quality control purposes for simultaneous analysis of these co-administered antigout drugs in their binary and ternary mixtures.

An innovative, simple, fast, specific and sensitive high performance liquid chromatographic method with ultraviolet detection (HPLC/UV) was established and validated for simultaneous determination of a combination of three commonly prescribed antigout drugs namely; Colchicine (CLN), Probenecid (PRD) and Febuxostat (FBX) in dosage forms and in human urine samples. GraceSmart RP C18 column was utilized for separation of the studied mixture using isocratic mode of mobile system consisting of acetonitrile: water (55: 45, v/v; containing 0.5% v/v formic acid). Flow rate and detection wavelengths programming were designed to obtain a rapid and efficient separation. The cited drugs were separated within 9 min. The retention times (tR) were 3.597, 5.357 and 8.250 for CLN, PRD and FBX; respectively. The linearity range for all the investigated drugs was 0.040–50.0 μg/mL with detection limits of 1.94–6.48 ng/mL. Additionally, the developed method was validated according to ICH and US-FDA guidelines and was successfully applied for simultaneous estimation of the studied drugs in their pure form, and in laboratory-made mixture solution of their respective tablets. The proposed method was also used for analysis of CLN and PRD in their combined tablets and in human urine samples obtained from healthy volunteers with good recoveries (98.39–101.87%). Furthermore, the stability of CLN-PRD mixture in urine samples was studied. In conclusion, this method is suitable for quality control purposes for simultaneous analysis of these co-administered antigout drugs in their binary and ternary mixtures.

A comprehensive review with 129 references for the analysis of commonly prescribed antigout drugs is presented. The review covers most of the methods described for the analysis of Febuxostat (FBX), Colchicine (CLN), and Probenecid (PRD) in pure forms, in different pharmaceutical dosage forms and in biological fluids. The review covers the period from 2000 till now.

A comprehensive review with 129 references for the analysis of commonly prescribed antigout drugs is presented. The review covers most of the methods described for the analysis of Febuxostat (FBX), Colchicine (CLN), and Probenecid (PRD) in pure forms, in different pharmaceutical dosage forms and in biological fluids. The review covers the period from 2000 till now.