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  本文選題：高效液相色譜法　切入點(diǎn)：氨基甲酸酯類(lèi)農(nóng)藥　出處：《河北大學(xué)》2012年碩士論文

【摘要】：隨著經(jīng)濟(jì)和社會(huì)的發(fā)展以及人們生活水平的提高，對(duì)食品的質(zhì)量要求也越來(lái)越高。由于近年來(lái)食品安全問(wèn)題時(shí)有發(fā)生，應(yīng)加強(qiáng)對(duì)食品質(zhì)量安全的檢測(cè)。本文第一章概括了氨基甲酸酯類(lèi)農(nóng)藥和植物生長(zhǎng)調(diào)節(jié)劑的性質(zhì)及危害，介紹了環(huán)境和食品中這兩類(lèi)物質(zhì)的主要分析檢測(cè)方法。第二章采用懸浮固化單液滴萃取的前處理方法，并結(jié)合高效液相色譜測(cè)定水中氨基甲酸酯類(lèi)農(nóng)藥，使用反相C18色譜柱（250mm×4.6mm i.d.,5μm），以甲醇－乙腈－水體系為流動(dòng)相（體積比為40:17:43）。對(duì)于水中速滅威，殘殺威，西維因，抗蚜威，葉蟬散，仲丁威六種氨基甲酸酯類(lèi)農(nóng)藥，檢出限為1-4ng/mL，加標(biāo)回收率在82.17%以上。實(shí)驗(yàn)考察了在懸浮固化單液滴萃取過(guò)程中，萃取劑種類(lèi)、液滴體積、萃取時(shí)間、攪拌速度、鹽析效應(yīng)及pH等對(duì)回收率的影響。第三章采用固相分散-高效液相色譜法測(cè)定番茄醬中的植物生長(zhǎng)調(diào)節(jié)劑。以無(wú)水硫酸鈉為分散劑，采用TOSOH C18柱（150×4.6mm，5μm）分離，以甲醇－水(體積比50:50)為流動(dòng)相，檢測(cè)波長(zhǎng)230nm。在0.005～5.0mg/L范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)大于0.999。兩組分方法檢出限均為0.02μg/g，平均回收率為87.0%和71.0%，相對(duì)標(biāo)準(zhǔn)偏差為1.7%和1.5%。第四章，探討了動(dòng)態(tài)固相微萃取-液相色譜法測(cè)定牛奶中的三種雌激素的可行性。使用聚丙烯微孔膜包封吸附劑，將其放入樣品中，攪拌萃取。使用Diamonsil C18柱（250mm×4.6mm，5μm）進(jìn)行分離；并以甲醇-乙腈-水體系（體積比為20：40：40）為流動(dòng)相；同時(shí)使用甲酸調(diào)節(jié)至pH=5；在波長(zhǎng)為230nm下檢測(cè)。炔雌醇，，己烯雌酚在1.0-100μg/mL，雙烯雌酚在0.5-100μg/mL的范圍內(nèi)線性良好，線性相關(guān)系數(shù)達(dá)到0.9996。
[Abstract]:With the development of economy and society and the improvement of people's living standard, the quality of food is becoming more and more demanding. The first chapter summarizes the properties and hazards of carbamate pesticides and plant growth regulators. The main analytical and detection methods of these two kinds of substances in environment and food were introduced. In chapter 2, the pretreatment method of suspension solidification single droplet extraction and the determination of carbamate pesticides in water by high performance liquid chromatography (HPLC) were used. A reversed-phase C18 column of 250mm 脳 4.6mm i.d. was used with methanol-acetonitrile-water system as mobile phase (volume ratio: 40: 17: 43). The detection limit is 1 ~ 4 ng / mL, and the recovery rate is more than 82.17%. The kinds of extractants, droplet volume, extraction time and agitation speed are investigated in the process of suspension solidification single droplet extraction. The effect of salting out and pH on the recovery. In chapter 3, the plant growth regulators in tomato paste were determined by solid phase dispersion and high performance liquid chromatography. The plant growth regulators were separated by TOSOH C18 column (150 脳 4.6 mm ~ 5 渭 m) with anhydrous sodium sulfate as dispersant. Using methanol-water (50: 50 volume ratio) as mobile phase, the detection wavelength was 230 nm 路m. The correlation coefficient was greater than 0.999.The detection limit of the two methods was 0.02 渭 g / g, the average recovery was 87.0% and 71.0%, and the relative standard deviation was 1.7% and 1.5. The feasibility of dynamic solid-phase microextraction (SPME) -liquid chromatography for the determination of three kinds of estrogens in milk was discussed. Polypropylene microporous membrane was used to encapsulate the adsorbents in the sample, and was agitated for extraction. Diamonsil C18 column (250mm 脳 4.6mm / 5 渭 m) was used for separation. The methanol-acetonitrile-water system (20: 40: 40 by volume) was used as mobile phase, adjusted to pH 5 by formic acid, and detected at wavelength of 230nm. The linearity of ethylestradiol and diethylstilbestrol was 1.0-100 渭 g / mL, and the linear correlation coefficient was 0.9996 in the range of 0.5-100 渭 g/mL for diethylstilbestrol.
【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2012
【分類(lèi)號(hào)】：R155.5;O657.72

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