Hassannejad, Mohammad, Alizadeh, Kamal, Mahboob, Nemati, Matin, Amir Abbas, Pourmohammad, Roya. (1403). Extraction and Quantification of 17-β-Estradiol in Wastewater Samples via Coacervative Phase Formation with β-Cyclodextrin and High-Performance Liquid Chromatography. فصلنامه علمی زیست فناوری گیاهان زراعی, 11(2), 173-181. doi: 10.30473/ijac.2025.74335.1318
Mohammad Hassannejad; Kamal Alizadeh; Nemati Mahboob; Amir Abbas Matin; Roya Pourmohammad. "Extraction and Quantification of 17-β-Estradiol in Wastewater Samples via Coacervative Phase Formation with β-Cyclodextrin and High-Performance Liquid Chromatography". فصلنامه علمی زیست فناوری گیاهان زراعی, 11, 2, 1403, 173-181. doi: 10.30473/ijac.2025.74335.1318
Hassannejad, Mohammad, Alizadeh, Kamal, Mahboob, Nemati, Matin, Amir Abbas, Pourmohammad, Roya. (1403). 'Extraction and Quantification of 17-β-Estradiol in Wastewater Samples via Coacervative Phase Formation with β-Cyclodextrin and High-Performance Liquid Chromatography', فصلنامه علمی زیست فناوری گیاهان زراعی, 11(2), pp. 173-181. doi: 10.30473/ijac.2025.74335.1318
Hassannejad, Mohammad, Alizadeh, Kamal, Mahboob, Nemati, Matin, Amir Abbas, Pourmohammad, Roya. Extraction and Quantification of 17-β-Estradiol in Wastewater Samples via Coacervative Phase Formation with β-Cyclodextrin and High-Performance Liquid Chromatography. فصلنامه علمی زیست فناوری گیاهان زراعی, 1403; 11(2): 173-181. doi: 10.30473/ijac.2025.74335.1318
1Faculty of Chemistry, Lorestan University, Khorramabad 6813717133, Iran
2Department of Pharmacology, Tabriz University of Medical Sciences, Tabriz 1476651664, Iran
3Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, Tabriz, Iran
4Department of Pathology, Tabriz University of Medical Sciences, Tabriz, Iran
چکیده
A simple, rapid, and cost-effective method for the determination of 17-β-estradiol in water samples was developed. The method is based on the extraction of the 17-β-estradiol–β-cyclodextrin complex using a coacervate phase composed of reverse micelles of decanoic acid, followed by high-performance liquid chromatography with ultraviolet detection for quantification. The effects of key parameters, including decanoic acid concentration (50–200 mg in a 30 mL total volume), tetrahydrofuran concentration (1–15% v/v), β-cyclodextrin to 17-β-estradiol molar ratio (1:1–1:4), ionic strength (0–1 M) NaCl, pH (1–4), and extraction time (0–30 min), on recoveries and enrichment factors were studied and optimized. The optimal extraction conditions involved stirring a 20 mL water sample containing 50 mg of decanoic acid with 3 mL of THF, using a 1:1 molar ratio of 17-β-estradiol to β-cyclodextrin complex, for 10 minutes, followed by centrifugation, 10 min at 4000 rpm. Recoveries and enrichment factors of 17-β-estradiol was primarily influenced by the decanoic acid and THF concentrations that form the coacervate phase but remained independent of the ionic strength of the sample solution. The recovery rate, enrichment factor, limit of detection, and relative standard deviation for 17-β-estradiol were 95%, 284, 0.19 μg/L, and 4.34%, respectively. This method was applied to analyze 17-β-estradiol in city water, mineral water, and pastewater samples. No 17-β-estradiol was detected in mineral water, while its concentration in city water and pastewater was found to be 1.9 μg/L and 33.67 μg/L, respectively.
استخراج و تعیین کمیت 17-β-استرادیول در نمونه های فاضلاب از طریق تشکیل فاز کواسرویتیو با -βسیکلودکسترین و کروماتوگرافی مایع با کارایی بالا
نویسندگان [English]
محمد حسن نژاد1؛ کمال علیزاده1؛ نعمتی محبوب2؛ امیرعباس متین3؛ رویا پورمحمد4
1دانشکده شیمی، دانشگاه لرستان، خرم آباد، کد پستی ۶۸۱۳۷۱۷۱۳۳، ایران
2گروه فارماکولوژی، دانشگاه علوم پزشکی تبریز، تبریز، کد پستی ۱۴۷۶۶۵۱۶۶۴، ایران
3گروه شیمی، دانشکده علوم، دانشگاه شهید مدنی آذربایجان، تبریز، ایران
4گروه پاتولوژی، دانشگاه علوم پزشکی تبریز، تبریز، ایران
چکیده [English]
یک روش ساده، سریع و مقرون به صرفه برای تعیین 17-β-استرادیول در نمونه های آب توسعه داده شد. این روش مبتنی بر استخراج کمپلکس 17-β-استرادیول- β-سیکلودکسترین با استفاده از یک فاز کواسروای متشکل از میسل های معکوس اسید دکانوئیک و به دنبال آن کروماتوگرافی مایع با کارایی بالا با تشخیص اشعه ماوراء بنفش برای تعیین مقدار است. اثرات پارامترهای کلیدی، از جمله غلظت اسید دکانوئیک (50 تا 200 میلی‌گرم در حجم کل 30 میلی‌لیتر)، غلظت تتراهیدروفوران (1-15 درصد حجمی)، نسبت مولی بتا سیکلودکسترین به 17-β-استرادیول (1:1-1:4)، قدرت یونی 0-1 مولارNaCl، pH 1-4 و زمان استخراج (0-30دقیقه) روی شرایط استخراج بهینه و فاکتور تغلیظ مطالعه شد. شرایط استخراج بهینه نمونه آب 20 میلی لیتری حاوی 50 میلی گرم اسید دکانوئیک با 3 میلی لیترTHF، با استفاده از نسبت مولی 17-β-استرادیول به 17-β-استرادیول (1:3) برای مدت 10 دقیقه و به دنبال آن سانتریفوژ 4000 دور در دقیقه بود 17-β-استرادیول در درجه اول تحت تأثیر غلظت اسید دکانوئیک و THF بود که فاز کواسروای را تشکیل می دهند، اما مستقل از قدرت یونی محلول نمونه باقی ماند. نرخ بازیابی، فاکتور غنی‌سازی، حد تشخیص و انحراف استاندارد نسبی برای 17--βاسترادیول به ترتیب 95 درصد ، 284، μg/L 0.19 و 4.34 درصد بود. این روش برای تجزیه و تحلیل 17-β-استرادیول در نمونه های آب شهری، آب معدنی و آب شیرین استفاده شد. هیچ 17-β-استرادیول در آب معدنی شناسایی نشد، در حالی که غلظت آن در آب شهری و آب شیرین به ترتیب 1.9 μg/L و 33.67 μg/L بود.
کلیدواژه‌ها [English]
17β-استرادیول, β-سیکلودکسترین, فاز میسلی, استخراج کواسروای, فاکتور غنی‌سازی
مراجع
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