Faculty Of Pharmacy Research Paper

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    On-line coupling of derivatization with pre-concentration to determine trace levels of methotrexate
    (Xi'an Jiaotong University, 2013) Emara S.; Masujima T.; Zarad W.; Kamal M.; El-Bagary R.; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Misr International University; Km 28 Ismailia Road; Cairo; Egypt; Analytical Molecular Medicine and Devices Laboratory; Hiroshima University; Graduate School of Biomedical Sciences; 1-2-3; Kasumi; Minami-ku; Hiroshima 734-8551; Japan; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; Modern Sciences and Arts University; 26 July Mehwar Road intersection with Wahat Road; 6 October City; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr El Aini St.; Cairo 11562; Egypt
    A new simple, sensitive and precise green analytical procedure using an automated packed-reactor derivatization technique coupled with on-line solid-phase enrichment (SPEn) has been developed and evaluated to determine trace levels of methotrexate (MTX). The method was based on injection of MTX into a flowing stream of phosphate buffer (0.04 M, pH 3.4), carried through the packed oxidant reactor of Cerium (IV) trihydroxyhydroperoxide for oxidative cleavage of the drug into highly fluorescent product, 2,4-diaminopteridine-6- carboxylic acid, followed by SPEn on a head of short ODS column (10 mm�4.6 mm i.d., 5 ?m particle size). The flow rate was 0.25 mL/min and packed reactor temperature was 40 �C. The trapped product was back-flush eluted from the ODS column to the detector by column-switching with an environmentally friendly mobile phase consisting of ethanol and phosphate buffer (0.04 M, pH 3.4) in the ratio of 5:95 (v/v). The eluent was monitored at emission and excitation wavelengths of 460 and 360 nm, respectively. The calibration curve was linear over the concentration range of 1.25-50 ng/mL with a detection limit of 0.08 ng/mL. The method was successfully applied to determine MTX in pharmaceutical formulations with mean percentage recovery ranging from 99.48 to 99.60. � 2013 Xi'an Jiaotong University.
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    On-line solid-phase enrichment coupled to packed reactor flow injection analysis in a green analytical procedure to determine low levels of folic acid using fluorescence detection
    (2012) Emara S.; Masujima T.; Zarad W.; Kamal M.; EL-Bagary R.; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Misr International University; Km 28 Ismailia Road; Cairo; Egypt; Analytical Molecular Medicine and Devices Laboratory; Hiroshima Univ.; Graduate School of Biomedical Sciences; 1-2-3; Kasumi; Minami-ku; Hiroshima; 734-8551; Japan; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; Modern Sciences and Arts University; 26 July Mehwar Road intersection with Wahat Road; 6 October City; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr El Aini St; Cairo; 11562; Egypt
    Background: Analysis of folic acid (FA) is not an easy task because of its presence in lower concentrations, its lower stability under acidic conditions, and its sensitiveness against light and high temperature. The present study is concerned with the development and validation of an automated environmentally friendly pre-column derivatization combined by solid-phase enrichment (SPEn) to determine low levels of FA.Results: Cerium (IV) trihydroxyhydroperoxide (CTH) as a packed oxidant reactor has been used for oxidative cleavage of FA into highly fluorescent product, 2-amino-4-hydroxypteridine-6-carboxylic acid. FA was injected into a carrier stream of 0.04 M phosphate buffer, pH 3.4 at a flow-rate of 0.25 mL/min. The sample zone containing the analyte was passed through the CTH reactor thermostated at 40�C, and the fluorescent product was trapped and enriched on a head of small ODS column (10 mm x 4.6 mm i.d., 5 ?m particle size). The enriched product was then back-flush eluted by column-switching from the small ODS column to the detector with a greener mobile phase consisting of ethanol and phosphate buffer (0.04M, pH 3.4) in the ratio of 5:95 (v/v). The eluent was monitored fluorimetrically at emission and excitation wavelengths of 463 and 367 nm, respectively. The calibration graph was linear over concentrations of FA in the range of 1.25-50 ng/mL, with a detection limit of 0.49 ng/mL.Conclusion: A new simple and sensitive green analytical procedure including on-line pre-column derivatization combined by SPEn has been developed for the routine quality control and dosage form assay of FA at very low concentration level. The method was a powerful analytical technique that had excellent sensitivity, sufficient accuracy and required relatively simple and inexpensive instrumentation. � 2012 Emara et al.; licensee Chemistry Central Ltd.
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    Online pre-column derivatization with chromatographic separation to determine folic acid
    (2013) Emara S.; Masujima T.; Zarad W.; Kamal M.; Ei-Bagary R.; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Misr International University; Km 28 Ismailia Road; Cairo; Egypt; Analytical Molecular Medicine and Devices Laboratory; Hiroshima University; Graduate School of Biomedical Sciences; 1-2-3; Kasumi; Minami-ku; Hiroshima; 734-8551; Japan; Pharmaceutical Analytical Chemistry Department; Faculty of Pharmacy; Modern Sciences and Arts University; 26 July Mehwar Road intersection with Wahat Road; 6 October City; Egypt; Pharmaceutical Chemistry Department; Faculty of Pharmacy; Cairo University; Kasr El Aini St.; Cairo 11562; Egypt
    A simple, sensitive, and selective online pre-column derivatization high-performance liquid chromatographic method was developed and validated for the first time to determine trace levels of folic acid (FA). An oxidant cerium (IV) trihydroxyhydroperoxide packed reactor was used for pre-column oxidation and was combined by column switching with a C18 analytical column for sample enrichment and separation. The method was based on oxidative cleavage of FA into highly fluorescence products, 2-amino-4-hydroxypteridine-6-carboxaldehyde and the corresponding 2-amino-4-hydroxypteridine-6-carboxylic acid, during the flow of 0.04 M phosphate buffer (pH 3.5) containing the analyte through packed reactor at a flow rate of 0.2 mL/min and 40�C. The fluorescent products were enriched on the head of the analytical column for the final separation. The separation was performed at room temperature using a mobile phase consisting of phosphate buffer (0.04 M, pH 3.5) and acetonitrile (90:10, v/v). The eluents were monitored at emission and excitation wavelengths of 463 and 367 nm, respectively. The method showed excellent recovery, precision and accuracy with detection limits of 0.067 ng/mL from 500 L of sample FA. The developed method was successfully applied to the determination of FA in pharmaceutical formulations and showed a recovery of 99.31% and a relative standard deviation of 1.72%. 2012 � The Author [2012].