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Samer Housheh ¹, Saleh Trefi ², M. Fawaz Chehna ²

Affiliations
1 Department of Quality Control and Pharmaceutical Chemistry, Al-Andalus University, Tartous, SY
2 Department of Quality Control and Pharmaceutical Chemistry, University of Aleppo, Aleppo, SY

Abstract

The objective of the present work was to separate, identify and characterize the degradation products of Prasugrel hydrochloride under hydrolytic and oxidative stress conditions according to the International Conference on Harmonization (ICH) guideline Q1A (R2). The drug degraded under acidic, basic, and oxidative stress. Five degradation products were formed, which were separated using preparative TLC. Mass fragmentation pathway of the drug was first established with the help of GC/MS studies. The degradation products were subjected to FTIR and 1H NMR studies. The obtained mass spectral data were employed to characterize the degradation products and assign structures. The degradation products were identified as 5-(2- cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2(3H)-one, 5-(2-cyclopropyl- 1-(2-fluorophenyl)-2-oxoethyl)-5,6,7,7a-tetrahydrothieno[3,2-c]pyridin-2(4H)-one, 2-acetoxy-5-(2-cyclopropyl- 1-(2-fluorophenyl)-2-oxoethyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine 5-oxide, 1-cyclopropyl-2-(2- fluorophenyl)ethane-1,2-dione and 4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl acetate.

Keywords

Stress Studies, Prasugrel Hydrochloride, GC/MS, FTIR, 1H NMR, Degradation Products.

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Aidaa Maaz ¹, Saleh Trefi ¹, Mohammad Haroun ², Wassim Abdelwahed ³

Affiliations
1 Department of Pharmaceutical Chemistry and Quality Control, Aleppo University, SY
2 Department of Pharmaceutical Chemistry and Quality Control, Alandalus University, SY
3 Department of Pharmaceutical Technology, Aleppo University, SY

Abstract

The purpose of the present study was to prepare microparticles containing Gatifloxacin suitable for ocular drug delivery. Polycaprolactone microparticles were prepared using the double emulsion (water-in-oil-in-water) solvent extraction/evaporation method. Two different modified methods were applied and the influence of their preparation parameters on the final microparticles properties was studied in an attempt to control particle sizes and encapsulation efficiency. By adjusting formulation and process parameters, we uncovered that using of 3% (w/v) PVA as emulsion stabilizer in the internal aqueous phase (first studied process) facilitated microparticles (77% of particles more than 100μm in size) which is suitable for oral drug delivery, but with highest entrapment efficiency EE% (82.12%). Whereas introducing 5% (w/v) of PVP as stabilizing agent and 5% (w/v) of NaCl as osmotic balancer in the external aqueous phase (second studied process) afford microparticles which is optimal in size for ophthalmic drug delivery (95% of particles less than 25μm in size) with an acceptable EE% (30.18%).The later result demonstrated that, this colloidal system could be developed in order to use as drug carriers for ocular drug delivery, which offers several advantages including longevity, stability and bioavailability of encapsulated drug. Moreover, it seemed to be applicable for sustained ocular drug delivery allowing minimizing dose repetition to reduce systemic side effects and enhance patient compliance.

Keywords

Gatifloxacin, Microparticles, Ocular Drug Delivery, Double Emulsion, PCL, PVA, PVP.

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Saleh Trefi ¹, Yaser Bitar ¹, Veronique Gilard ²

Affiliations
1 Pharmaceutical Quality and Pharmaceutical Chemistry Department-University of Aleppo, SY
2 Laboratoire SPCMIB (UMR CNRS 5068), Université Paul Sabatier, Université de Toulouse, 118 route de Narbonne, 31062 Toulouse cedex, FR

Abstract

The objective of this study was to develop and validate a new ion-pair reversed phase high performance liquid chromatographic method on a standard C18-type stationary phase with UV detection for the analysis of the recent two-drugs combination sacubitril/valsartan in tablets. The mobile phase consisted of a mixture of 45% of 10-3 M of cetyltrimethylammonium bromide (cetrimide) as the ion-pairing agent and 55% acetonitrile. The method validation was based on linearity, accuracy, precision, robustness and specificity. This method exhibits good linearity and accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products. These results indicates that the proposed method is simple and applicable for the separation and determination of sacubitril, valsartan combination in tablets and could be a relevant method to implement in quality control laboratories.

Keywords

HPLC, Ion Pair Liquid Chromatography, Sacubitril, Valsartan.

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Muhamad Esam Kaf Alghazal ¹, Fadi Alrouh ², Yaser Bitar ¹, Saleh Trefi ¹

Affiliations
1 Pharmaceutical Quality and Pharmaceutical Chemistry Department – University of Aleppo, SY
2 Organic Chemistry Department– University of Al-Hawash, SY

Abstract

A specific and highly sensitive gas chromatographic method was developed for the simultaneous determination of chlorpheniramine maleate and dimenhydrinate using one drug as internal standard for the other one. The chromatographic conditions are aTRB-5-625 capillary column (60m × 0.25 mm i.d0.25μm film thickness) and nitrogen as a carrier gas at a flow rate of 1.0 mL min. The oven temperature was programmed at 230°C for 1 min, with a rise of 20°C min up to 250°C (held for 7 min). The injector and detector port temperatures were maintained at 290°C. Detection was carried out using flame ionization detector. Results of assay and recovery studies were statistically evaluated for its accuracy and precision using one drug as internal stander for the other one and vice versa. Objective: The objective of this study was to develop and validate a gas chromatographic method to separate and assay to antihistamine drugs, dimenhydrinate and chlorpheniramine maleate in pharmaceutical forms. This method was a practical additional choice in quality control laboratories.

Keywords

Chlorpheniramine Maleate, Dimenhydrinate, Gas Chromatography.

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