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Extraction Of Pyrethroids And Sudan From Liquid Samples

Posted on:2013-01-30Degree:MasterType:Thesis
Country:ChinaCandidate:S SunFull Text:PDF
GTID:2231330371485249Subject:Analytical Chemistry
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There are200kinds of nutritional components in wine which are beneficial forhuman health, such as carbohydrates, organic acid, amino acid, vitamin, inorganic saltand so on. These components are essential for human mental deterioration. There arephenolic substances in wine which have antioxidant function, and can present andcontrol degenerative diseases, such as aging, cataract, immunodepression and somecancers. Resveratrol found in seeds and skins of grape can caret cancer, resistinfection, and prolong human’s lifetime. There are many antidiabetic compounds inwine. If you drank wine in moderation, the risk of type2diabetes mellitus can belowered. Besides, because pH values of wine are2~2.5, which are similar with theseof gastric juice, so wine can promote digestion, increase appetite, lower blood lipids,soften vascular and so on. Due to health care effect of wine, wine received more andmore people’s attention. In recent years, the need of wine is increasing year after year,so people focus on the quality of wine. There are two parts in the thesis: the extractionof pyrethroids in red wine by MAMSPD, and the extraction of sudan in red wine andfruit juice by ionic liquid-based LLME.The pyrethroids in red wine were extracted and determined by MAMSPD-HPLC.The operational parameters, including the type and amount of adsorbents, the type andvolume of the elution solvent, extraction temperature and time were optimized. Therecoveries of the target analytes at80and400ng/mL-1levels from different winesamples were97.28~107.23%(RSD≤7.83) for bifenthrin,88.10~107.32%(RSD≤9.10) for permethrin,90.90~102.38%(RSD≤7.06) for lambda-Cyhalothrin,89.24~106.26%(RSD≤7.23) for deltamethrin, the limits of detection were3.6~8.8ng/mL, which can content the requests of some directives (e.p. EuropeanUnion Council Directive n.93/57/EEC). The target analytes were adsorbed onthe adsorbent under microwave irradiation instead of grinding in this proposedmethod. The extraction system was simple and the operation was easy. So it seemspossible to extend this method to the extraction of the other analytes in other liquidsamples by varying the extraction conditions. Ionic liquid based liquid-liquid microextraction (LLME) coupled with HPLCdetection has been developed for determination of sudan dyes in red wine and fruitjuice. In study, we have found the best conditions:50μL of [C6MIM][PF6], extractiontime (vigorously shaken with hand) is10min, pH=7, the NaCl concentration is5%.When the target analyte concentrations are80and400ng/mL-1, the extractionrecoveries for the analytes in red wine and friut samples are86.79–108.28%(RSD≤6.29)and68.54–85.66%(RSD≤6.19), respectively. The recoveries shouldbe acceptable, but the recoveries of the analytes in red wine samples are higher thanthose in the fruit juice samples. Because red wine containes some ethanol which canbe used as the dispersant, the ionic liquid droplets in wine should be smaller thanthose in fruit juice, so the recoveries analytes in wine are higher. In this method, thelimits of detection were0.428ng/mL for sudanⅠ,0.938ng/mL for sudanⅡ,1.334ng/mL for sudan Ⅲ,1.454ng/mL for sudanⅣ, respectively. Compared withconventional liquid-liquid extraction (CLLE) and ultrasonic extraction (UE), whenLLME was applied, the sample amount was less (LLME:4mL; CLLE:10mL; UE:10mL), the extraction time was shorter (LLME:15min; CLLE:110min; UE:50min)and the extraction solvent amount was less (LLME:0.05mL IL; CLLE:15mL hexane;UE:20mL hexane), while enrichment factor was higher(160-189). The limits ofdetection were0.428-1.454ng/mL. The proposed method offers a simple, rapid andefficient sample preparation for determining sudan dyes in red wine and fruit juicesamples.
Keywords/Search Tags:Microwave-assisted extraction (MAE), Matrix solid-phase dispersion extraction(MSPD, Liquid-liquid microextraction (LLME), Ionic liquid, Red wine
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