استخراج و تعیین مقدار گروهی از ترکیبات آلی فرار با روش میکرواستخراج فاز جامد از فضای فوقانی- کروماتوگرافی گازی در نمونه های چای و سبزیجات
محورهای موضوعی : فصلنامه کیفیت و ماندگاری تولیدات کشاورزی و مواد غذایی
محبوبه دهقانی
1
,
مریم کاظمی پور
2
,
مهدی انصاری
3
,
مهدی شهیدی زندی
4
1 - دانشجوی دکتری، گروه شیمی تجزیه، واحد کرمان، دانشگاه آزاد اسلامی، کرمان، ایران
2 - استاد، گروه شیمی تجزیه، واحد کرمان، دانشگاه آزاد اسلامی، کرمان، ایران
3 - استاد، گروه کنترل دارو و غذا، دانشکده داروسازی، دانشگاه علوم پزشکی کرمان، کرمان، ایران
4 - دانشیار، گروه شیمی تجزیه، واحد کرمان، دانشگاه آزاد اسلامی، کرمان، ایران
کلید واژه: میکرواستخراج فاز جامد, نانو لوله های کربنی, کروماتوگرافی گازی, جاذب کامپوزیتی, هیدروکربن های آروماتیک,
چکیده مقاله :
در این پژوهش، یک جاذب کامپوزیتی از پلی پیرول، نانولوله های کربنی چند جدارۀ اصلاح شده و کربن فعال اصلاح شده حاصل از پوستۀ سخت فندق، به روش الکتروشیمیایی سنتز و از آن برای تجزیۀ گروهی از هیدروکربن های آروماتیک فرار در نمونه های چای و سبزیجات استفاده شد. بهینه سازی پارامترهای مؤثر بر فرآیند پوشش دهی فیبر و هچنین پارامترهای مؤثر در مرحله واجذبی آنالیت ها به روش کلاسیک و مرسوم تغییر یک متغیر در یک زمان (OVAT)، انجام شد. بر اساس نتایج حاصله پتانسیل پوشش دهی 1 ولت، زمان پوشش دهی 1000 ثانیه، دمای واجذبی 280 درجه سانتی گراد و زمان واجذبی 5 دقیقه بعنوان مقادیر بهینه در نظر گرفته شدند. برای بهینه سازی پارامترهای مؤثر در مرحله استخراج از طراحی آزمایش استفاده شد که در نهایت دمای استخراج 25 درجه سانتی گراد، زمان استخراج 30 دقیقه و مقدار نمک 10 درصد بدست آمد. در روش پیشنهادی، منحنی کالیبراسیون بدست آمده برای نفتالن در محدودۀ غلظتی 8-5/0 میکروگرم بر لیتر، برای فلورن و فنانترن در محدودۀ غلظتی 15-2 میکروگرم بر لیتر و برای آنتراسن و پایرن در محدودۀ غلظتی10-2 میکروگرم بر لیتر خطی بود. در شرایط بهینه، حدود تشخیص برای آنالت های هدف 9/0-06/0 میکروگرم بر لیتر بود و تکرارپذیری (%RSD)، روش در محدودۀ 6/8-5/0 متغییر بود.
In this study, a composite coating of polypyrrole/modified multiwalled carbon nanotubes/modified activated carbon prepared from hazelnut shells (PPy/MWCNTs/AC), was electrochemically synthesized and used for analyzing a group of volatile aromatic hydrocarbons in tea and vegetable samples. In order to obtain an adherent and stable composite coating, the effective parameters on electrodeposition process were optimized using the one-variable-at-a-time procedure, as well as the effective parameters in the desorption step of analytes was performed by this method. Based on the results, the deposition potential of 1 V, the deposition time of 1000 seconds, the desorption temperature of 280 ° C and the desorption time of 5 minutes were considered as the optimal values. To optimize the effective parameters in the extraction stage, the experimental design was used. Finally, the extraction temperature was 25 ° C, the extraction time was 30 minutes and the amount of salt was 10%. The calibration curve for each analyte in a range was linear as follows: 2 ̶ 15 µg ̸ L (fluorene and phenanthrene), 2 ̶ 10 µg ̸ L (anthracene and pyrene) and 0.5 ̶ 8 µg ̸ L (naphthalene). Under the optimized conditions, the amounts of the detection limits (LODs) calculated at S ̸ N proportion of 3, were varied from 0.06 to 0.9 µg ̸ L. The RSDs% of the peak areas ranged between 0.5 and 8.6%.
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