食品和水中氨基甲酸酯农药及植物激素的液相色谱分析

发布时间：2018-03-29 08:15

本文选题：高效液相色谱法　切入点：氨基甲酸酯类农药　出处：《河北大学》2012年硕士论文

【摘要】：随着经济和社会的发展以及人们生活水平的提高，对食品的质量要求也越来越高。由于近年来食品安全问题时有发生，应加强对食品质量安全的检测。本文第一章概括了氨基甲酸酯类农药和植物生长调节剂的性质及危害，介绍了环境和食品中这两类物质的主要分析检测方法。第二章采用悬浮固化单液滴萃取的前处理方法，并结合高效液相色谱测定水中氨基甲酸酯类农药，使用反相C18色谱柱（250mm×4.6mm i.d.,5μm），以甲醇－乙腈－水体系为流动相（体积比为40:17:43）。对于水中速灭威，残杀威，西维因，抗蚜威，叶蝉散，仲丁威六种氨基甲酸酯类农药，检出限为1-4ng/mL，加标回收率在82.17%以上。实验考察了在悬浮固化单液滴萃取过程中，萃取剂种类、液滴体积、萃取时间、搅拌速度、盐析效应及pH等对回收率的影响。第三章采用固相分散-高效液相色谱法测定番茄酱中的植物生长调节剂。以无水硫酸钠为分散剂，采用TOSOH C18柱（150×4.6mm，5μm）分离，以甲醇－水(体积比50:50)为流动相，检测波长230nm。在0.005～5.0mg/L范围内线性关系良好，相关系数大于0.999。两组分方法检出限均为0.02μg/g，平均回收率为87.0%和71.0%，相对标准偏差为1.7%和1.5%。第四章，探讨了动态固相微萃取-液相色谱法测定牛奶中的三种雌激素的可行性。使用聚丙烯微孔膜包封吸附剂，将其放入样品中，搅拌萃取。使用Diamonsil C18柱（250mm×4.6mm，5μm）进行分离；并以甲醇-乙腈-水体系（体积比为20：40：40）为流动相；同时使用甲酸调节至pH=5；在波长为230nm下检测。炔雌醇，，己烯雌酚在1.0-100μg/mL，双烯雌酚在0.5-100μg/mL的范围内线性良好，线性相关系数达到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.
【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R155.5;O657.72

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