میکرواستخراج و اندازه¬گيري کوله کالسیفرول (ویتامین D3) در سیالهای زیستی با یک روش سه فازی و بهکارگیری فیبر توخالی و دو حلال آلی امتزاج‌ناپذیر
محورهای موضوعی : شیمی تجزیه
1 - استادیار شیمی تجزیه، دانشکده شیمی، واحد تهران شمال، دانشگاه آزاد اسلامی، تهران، ایران.
کلید واژه: ویتامین D3, سوانگاری مايع با کارايي بالا, فيبر توخالي, سیالهای زیستی, پیش‌تغلیظ.,
چکیده مقاله :
در این مطالعه، استخراج و اندازهگیری ویتامین D3 در سیالهای زیستی با روش میکرواستخراج مایع-مایع با فیبر توخالی انجام شد. بدین‌منظور از روش سه فازی و بهکارگیری دو حلال آلی امتزاج‌ناپذیر در دیواره و درون فیبراستفاده شد. ویتامین از 8 میلیلیتر محلول نمونه با لایه نازکی از یک حلال آلی (نرمال دودکان) که در منافذ فیبر قرار دارد، استخراج شد. سپس، در داخل فیبر که حاوی استونیتریل درمقیاس میکرولیتر بود، استخراج برگشتی انجام شد. عوامل موثر بر این روش بررسی و شرایط بهینه بهدست آمد. در این شرایط عامل غنیسازی 130، حدتشخیص ng ml-1 9/0 و نمودار واسنجی در گستره 3 تا ng ml-1 1000 با R2 برابر با 999/0 بهدست آمد. برای بررسی دقت روش پیشنهادشده، تکرارپذیری در یک روز و تکثیرپذیری در چند روز انجام شد و انحراف معیار نسبی به ترتیب 4/5 و 1/6 بهدست آمد. در ادامه برای اثبات توانمندی روش پیشنهادی، استخراج این ویتامین از سیالهای زیستی انجام شد و با پژوهشهای انجام‌شده مقایسه شد و نتیجههای قابل‌قبولی بهدست آمد.
The validation of hollow fiber based on using two immiscible organic solvents in the lumen and wall pores of hollow fiber was evaluated for extraction and preconcentration of a trace amount of vitamin D3, before determination by HPLC-UV technique. The analyte was extracted from an 8-ml sample solution, into a thin layer of an organic solvent (n-dodecane) impregnated in hollow fiber pores, and finally back-extracted into an organic solvent (acetonitrile) located inside the lumen of the hollow fiber. The factors affecting the HF-LLLME of the target analyte were investigated and the optimal extraction conditions were determined. Under optimized conditions, the enrichment factor of 130 and limit of detection (LOD) of 0.9 ng ml-1 were obtained. The calibration curve was linear within the range of 3 to 1000 ng ml-1 with reasonable linearity (R2 = 0.999). The percent relative within-day and between-day standard deviation (RSD %) were 5.4 and 6.1, respectively. Finally, the feasibility of the proposed method was successfully evaluated by extraction and determination of the analyte in the biological fluids, and satisfactory results were obtained.
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