عنوان:توسعه و معتبرسازی روش الكتروفورز موئین تلفیق شده با تكنیکهای نوينمیكرو استخراج بر پايهی فناوری نانو به منظور آنالیز برخی از داروهای خوراكیشیمیدرمانی در نمونههای خون بیماران مبتال به سرطانهای دستگاه گوارشی
Development and validation of capillary electrophoresis method coupledwith novel nano-based microextraction techniques for analysis of someorally-administered chemotherapy drugs in blood samples from patients with gastrointestinal cancers
- Tez No: 768632
- Danışmanlar: DR. REZA MALEKZADEH
- Tez Türü: Doktora
- Konular: Gastroenteroloji, Onkoloji, Gastroenterology, Oncology
- Anahtar Kelimeler: Capillary electrophoresis, Orally-administered chemotherapy drugs, Determination, Validation, Sample preparation, Nanotechnology, Biological samples, Cancer
- Yıl: 2017
- Dil: Arapça
- Üniversite: Urmia University
- Enstitü: Yurtdışı Enstitü
- Ana Bilim Dalı: Belirtilmemiş.
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 247
Özet
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Özet (Çeviri)
Capillary electrophoresis (CE) has been used increasingly more over the last decade in the area of medicinal and drug analysis. Numerous pharmaceutical products and prodrug components have been analyzed using this technique because of its high efficiency and short separation times in comparison with other chromatographic techniques. However, the inherent lack of detection sensitivity in CE-based techniques especially in complex bio-matrices is one of the contributing factors to the limited development on CE in this particular area of bioanalysis. In this project, the potential of CE as a tool in the analysis and determination of some widely used orally-administered chemotherapy drugs in blood samples from patients with gastrointestinal cancers was investigated. The purpose of the first part of present study is development and validation of a simple, novel, selective and fast off-line microextraction technique combining capillary electrophoresis with in-column filed-amplified sample injection (FASI) for simultaneous determination of capecitabine (CAP) and its active metabolite, 5-Flourouracil (5-FU), in human plasma. At the moment, there is a lack of using cost-effective CE tool combined with novel nanotechnology-based sample clean-up/preconcentration techniques for simultaneous analysis of these important anti-cancer agents in plasma samples. This research intends to fill this gap and describe a simple off-line sample pretreatment by means of AgNPs@MCM-41 reinforced HF-solid/liquid phase microextraction (AgNPs@MCM41-HF-SLPME) with subsequent quantitation by FASI-CE. The separation of analytes was performed using a BGE containing 60 mM phosphate-Tris buffer (pH 7) with 10% (v/v) methanol as an organic modifier. Various parameters affecting the off-line microextraction efficiency as well as FASI were optimized. The linearity, sensitivity, precision, accuracy, recovery, selectivity, specificity, stability as well as the robustness of the method was evaluated from spiked human plasma samples during the course of validation. The results revealed that the presented analytical technique demonstrates acceptable accuracy and precision, miniaturized sample preparation and a reduced need for complicated equipment along with an acceptable analysis time. The validated method is successfully applied to determine CAP and 5-FU in plasma samples obtained from the patients who received CAP. The focus of the second part of this study is development of a new, convenient, rapid and sensitive electro-membrane extraction approach (based on an ionic liquid-supported MWCNTs/ZnO reinforced hollow fiber, for the first time) as an off-line sample cleanup/preconcentration method coupled with capillary electrophoresis (CE) using field-amplified sample injection (FASI) for quantification of Imatinib mesylate in human plasma. The nanohybrid sorbent, coated by 1-octyl-3-methylimidazolium bromide ionic liquid ([OMIm]Br) in this research, was prepared by a feasible basic catalyzed sol-gel method. Then, it was immobilized (supported by capillary forces and sonication) in pores of a segment of a polypropylene hollow fiber membrane as the extraction unit after dispersing in 2-nitrophenyl octyl ether (NPOE) solvent and subsequently served as the supported liquid membrane (SLM) composition. Significant variables affecting the proposed method were evaluated and optimized to achieve the maximum extraction performance. The developed method was validated according to FDA guidelines. Regarding the validation results, the method is proved to be linear (R2 =0.998) over concentrations ranging from 20 to 1500 ng mL-1 . The mean RSD values for intra- and inter-day precision studies were 6.83 and 7.71%, respectively. Finally, the validated method was successfully applied to determine Imatinib mesylate in patient's plasma samples.
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