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دندریمرهای پلی آمیدوآمین اصلاح شده با نانوذرات مغناطیسی به عنوان جاذب برای ریز استخراج فاز جامد مغناطیسی همزمان میکونازول، کلوتریمازول و تیکونازول و اندازه گیری با دستگاه کروماتوگرافی مایع با کارآیی بالا | ||
| شیمى کاربردى روز | ||
| دوره 18، شماره 69، دی 1402، صفحه 45-56 اصل مقاله (897.74 K) | ||
| نوع مقاله: مقاله علمی پژوهشی | ||
| شناسه دیجیتال (DOI): 10.22075/chem.2023.30294.2165 | ||
| نویسندگان | ||
| محسن شیرخدای کاشانی1؛ سید مهدی قریشی1؛ میلاد غنی* 2؛ بهروز ملکی3 | ||
| 1گروه شیمی تجزیه، دانشکده شیمی، دانشگاه کاشان، کاشان، ایران | ||
| 2گروه شیمی تجزیه، دانشکده شیمی، دانشگاه مازندران، بابلسر، ایران | ||
| 3گروه شیمی آلی، دانشکده شیمی، دانشگاه مازندران، بابلسر، ایران | ||
| تاریخ دریافت: 17 فروردین 1402، تاریخ بازنگری: 14 اردیبهشت 1402، تاریخ پذیرش: 20 آبان 1402 | ||
| چکیده | ||
| در این مطالعه، یک جاذب جدید بر اساس نسل دوم پلی (آمیدوآمین) مغناطیسی پوشش داده شده با سیلیس Fe3O4@SiO2@PAMAM))سنتز شد. . سپس، از میکروسکوپی الکترون روبشی با گسیل اثر میدانی (FE-SE)، طیف‌بینی پراش پرتوی ایکس (XRD)، طیف بینی مادون قرمز - تبدیل فوریه (FT- IR) ،آنالیز حرارتی وزن سنجی (TGA)، میکروسکوپ الکترونی عبوری (TEM) برای بررسی ریخت‌شناسی و ساختاری جاذب تهیه‌شده، استفاده گردید. برای بررسی کارآیی روش، میکونازول، کلوتریمازول و تیکونازول به‌عنوان سه گونه‌ی آزمایشی هدف انتخاب شدند و به منظور بررسی کارآیی روش پیشنهادی در آنالیز نمونههای حقیقی، نمونههای بیولوژیکی، مانند: ادرار و پلاسما مورد ارزیابی قرارگرفتند. تحت شرایط بهینه، گستره‌ی خطی غلظتی برای میکونازول دربازه‌ی µg L-1 1-200،برای کلوتریمازول در بازه‌ی µg L-1 1-500 و برای تیکونازول در بازه‌ی µg L-1 1-200 با ضریب تعیین (2r) دربازه‌ی 9871/0 تا 9977/0 در اندازه‌گیری آن‌ها توسط HPLC-UV محاسبه شدند. LOD روش برای میکونازول، کلوتریمازول و تیکونازول، به ترتیب µg L-116/0، µg L-118/0 و µg L-1 14/0 و LOQ روش نیز برای برای میکونازول، کلوتریمازول و تیکونازول ، به ترتیب µg L-1 53/0، µg L-1 60/0 وµg L-1 46/0 محاسبه گردیدند. RSD% روش در یک روز برای گونه‌های مورد بررسی در محدوده‌ی 9/5-6/4 برآورد شدند. | ||
| کلیدواژه‌ها | ||
| استخراج فاز جامد مغناطیسی؛ دندریمر پلی آمیدو آمین؛ داروهای ضد قارچ؛ کروماتوگرافی مایع با کارایی بالا؛ طراحی آزمایش | ||
| عنوان مقاله [English] | ||
| Dendritic Poly (amidoamine) Functionalized with Magnetic Nanoparticles as Sorbent for Simultaneous Magnetic Solid-Phase Extraction of Miconazole, Clotrimazole and Tioconazole Followed by Determination via HPLC-UV | ||
| نویسندگان [English] | ||
| Mohsen Shirkhodayekashani1؛ Sayed Mehdi Ghoreishi1؛ Milad Ghani2؛ Behrooz Maleki3 | ||
| 1Department of Analytical Chemistry, Faculty of Chemistry, University of Kashan, Kashan, Iran | ||
| 2Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran | ||
| 3Department of Organic Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran | ||
| چکیده [English] | ||
| In this study, an attempt was made to synthesize a new sorbent based on the second generation of silica coated magnetic poly(amidoamine) (Fe3O4@SiO2@PAMAM) to improve the performance of magnetic solid phase extraction (MSPE) of some antifungal drugs including miconazole, clotrimazole and ticonazole in various real samples such as urine and human plasma. The extracted analytes were measured by high performance liquid chromatography equipped with ultraviolet detection (HPLC-UV). Field emission-scanning electron microscopy (FE-SEM), X-ray diffraction analysis (XRD), Thermogravimetric analysis (TGA), Transmission electron microscopy (TEM) and Fourier transform-infrared spectroscopy (FT-IR) were used to study the morphology and structure of the prepared sorbent. The various factors such as: extraction time, sorbent amount, solvent desorption volume, desorption time, ionic strength and pH were studied and optimized. The method is validated according to ICH guidelines with respect to precision, accuracy, linearity, specificity, robustness, and limits of detection and quantification. Under the optimized condition, the linearity of the method was in the range of 1–500 µg L-1 (miconazole= 1-200 µg L-1, clotrimazole = 1-500 µg L-1 and ticonazole = 1-200 µg L-1). The obtained correlation coefficients (r^2) were between 0.9871-0.9977. The limits of detection (LODs) were also calculated to be 0.14-0.18 µg L-1 (miconazole= 0.16 µg L-1, clotrimazole = 0.18 µg L-1 and ticonazole=0.14 µg L-1). The limits of quantification (LOQs) were also in the range of 0.46-0.60 µg L-1 for the selected analytes. The relative standard deviations (RSDs%), were obtained in the range of 4.6 to 5.9%. Moreover, the calculated enrichment factors were between 85 and 93. The proposed method was also employed for the analysis of various real samples such as urine and plasma samples. The obtained recoveries indicated that the method was useful and applicable in complicated real samples | ||
| کلیدواژه‌ها [English] | ||
| Magnetic solid phase extraction, PAMAM, Antifungal, HPLC, Response surface methodology | ||
| مراجع | ||
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