食品安全用色谱法测定农药残留

Nataliia Tereshchenko, О. Kursenko, О. Khyzhan, O. Khyzhan, Oleksandr Bobunov, Lidiia Kovshun
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引用次数: 1

摘要

本文介绍了油籽、生菜、苹果样品的制备方法,并对苯并咪唑衍生物、苯胺嘧啶衍生物、联吡啶衍生物等化学类农药进行了色谱控制。考虑以下过程的实施:样品的均质化,通过固相或液-液萃取纯化提取物,获得植物提取物,获得分析物的提取物。葵花籽细粒均质样品,原料与萃取剂的最佳比例为1:20,苹果果糊状均质样品为1:10,生菜均质液体样品为1:5。分析系统中异种生物的分布辛烷/水,溶剂的偶极矩允许确定萃取剂能够溶解和去除原料中的异种生物。发现苯并咪唑类衍生物和苯胺嘧啶类衍生物的提取应采用乙腈与甲醇(4:1)的混合物,联吡啶类衍生物的提取最好采用甲醇三氟乙酸(9.5:0.5)。从人工富集的样品中提取的提取物中定量分析了外源物的含量。从含有微量脂肪的植物产品样品中除去了最完整的异种生物。样品制备中最困难的工序是提取葵花籽提取物的过程。从人工富集分析物的样品中提取的提取物中所含的异种生物制剂受提取过程发生的温度和提取时间的影响。根据样品基质的化学成分和分析物列表,提出了该方法可变组分的条件:在选择性溶剂的作用下获得植物提取物,在提取系统中以180-200 rpm恒定搅拌均匀的原料-溶剂,或在频率为37 kHz的超声波振动作用下从4°C到25°C,持续5-25分钟。采用高效液相和气相色谱法(液相和气相)和质量选择检测器对所研究植物提取物和分析物提取物的定性和定量组成进行控制。
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Determination of pesticide residues by chromatographic methods for food safety
The paper presents the methodology of preparation of samples of oilseeds, lettuce, apples for research by chromatographic control of xenobiotics of the following chemical groups of pesticides: benzimidazole derivatives, anilinopyrimidine derivatives, bipyridylium derivatives. The implementation of the following processes is considered: homogenization of the sample, purification of the extract by solid-phase or liquid-liquid extraction, obtaining a plant extract, obtaining an extract of analytes. For fine-grained homogenized samples of sunflower seeds, the optimal ratio of raw material -extragent is 1:20, for pasty homogenized samples of apple fruit - 1:10, for liquid samples of homogenized lettuce - 1: 5. Analysis of the distribution of xenobiotics in the system octane/water, the dipole moment of solvents allowed to determine the extractants that are able to dissolve and remove xenobiotics from raw materials. It was found that a mixture of acetonitrile and methanol (4: 1) should be used to remove benzimidazole derivatives and anilinopyrimidine derivatives, bipyridylium derivatives are best extracted with methanolic trifluoroacetic acid (9.5: 0.5). Quantitative analysis of xenobiotics content in extracts obtained from samples artificially enriched with xenobiotics was performed. The most complete xenobiotics were removed from samples of plant products containing traces of fat. The most difficult process of sample preparation is the process of obtaining sunflower seed extract. The content of xenobiotics in extracts obtained from samples artificially enriched in analytes is influenced by the temperature at which the process takes place and the duration of extraction. Based on the chemical composition of the sample matrix and the list of analytes, the conditions of the variable component of the methodology are proposed: obtaining plant extract under the action of selective solvents, homogenized raw material-solvent with constant stirring of the extraction system at 180-200 rpm, or under the action of ultrasonic vibrations with a frequency of 37 kHz from 4°C to 25°C for 5-25 minutes. The control of the qualitative and quantitative composition of the studied plant extracts and analyte extracts was investigated by the methods of high-performance liquid and gas chromatography (liquid and gas) with mass-selective detectors.
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