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Document Type |
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Thesis |
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Document Title |
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Development and Validation of Organic Derivatization Reagents for Chromatographic Analysis التطوير والتحقق من تحليل مشتقات الكواشف العضوية باستخدام الكروماتوجرافيا |
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Subject |
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Faculty of Science |
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Document Language |
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Arabic |
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Abstract |
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In this thesis, the analytical sensitivity of bisoprolol (BIS) and vildagliptin (VIL) was enhanced at the electrospray-ionization (ESI) source. 3-Bromomethyl-propyphenazone (BMP) was used as a derivatization reagent to improve the ESI sources ionization efficiency. The targeted analytes were analyzed in the serum of rats at a picogram level. The two compounds were coupled entirely with the BMP reagent, and the detection sensitivity of these derivatized analytes was matched with the untreated intact compounds at the same concentration level. Moreover, both BIS and VIL were labeled with dansyl chloride (Dns-Cl), and the resulting sensitivity was matched versus those derivatized with BMP. The chromatographic separation conditions, reaction variables, and mass spectrometry conditions were optimized. The stability of the formed derivatives was investigated. Rat serum samples were extracted using Sep-Pak Vac C18-100 mg columns and valsartan as an internal standard. Matrix effect at electrospray ionization -MS was studied for both BMP and Dns-Cl. The method was validated to include linearity and range, detection and quantification limits (LOD and LOQ), precision (% RSD), accuracy (% Er), recovery (% R), and stability. The linearity was examined on the spiked serum derivatized samples. Due to the reagent, ionization suppression at the ESI-MS ionization source was evaluated using the direct infusion method. The method was applied to rat serum after administering a single dose of BIS and VIL separately, and samples were collected at specific time intervals ranged from 0 to 8 hours. The plasma curve and the pharmacokinetic parameters were calculated. |
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Supervisor |
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Prof. Dr. Saleh Omar Bahaffi |
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Thesis Type |
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Doctorate Thesis |
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Publishing Year |
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1443 AH
2022 AD |
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Co-Supervisor |
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Prof. Dr. Alaa Eldin Mahmoud Khedr |
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Added Date |
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Saturday, January 28, 2023 |
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Researchers
| هدى عبد العزيز شاهين | Shaheen, Huda Abdulaziz | Researcher | Doctorate | |
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