新型微萃取技术在农药残留前处理中的应用
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摘要
氨基甲酸酯和有机磷类杀虫剂广泛应用于提高农业产量,对于提高农产品产量和质量有着重要意义。虽然这些农药能够有效提高农业产量和降低城市草坪等的维护成本,但是由于食物链的生物富集结果可能会影响到人类健康。传统的氨基甲酸酯和有机磷农药残留分析方法如液液萃取、固相萃取等,溶剂使用量大、前处理时间长,对环境容易造成二次污染,因此,对于氨基甲酸酯和有机磷农药残留的检测,需要寻求一种高效、快速的方法。
单滴液相微萃取、扩散微萃取、分子印迹固相萃取正是在这样情况下产生的新型样品前处理技术。单滴液相微萃取主要基于被分析物在微量进样器的针尖悬滴和水样体系之间的分配系数的不同;扩散微萃取的特点在于萃取溶剂充分扩散到水样中,获得极大的比表面积,使得被分析物能够在较短的时间内完成传质过程;分子印迹固相萃取具有特异的识别能力,并且相比于传统的固相萃取,能够重复使用。论文分别使用这三种先进的前处理技术,对氨基甲酸酯和有机磷农药残留前处理考察,主要研究内容有:
1.提出了单滴液相微萃取对氨基甲酸酯和有机磷农药残留同时测定的新方法,使用气相色谱质谱联用法分析,测定了水体中的氨基甲酸酯和有机磷农药残留。考察了影响萃取的各种因素,如萃取剂种类和用量、萃取时间、pH值、离子强度,最终确定了最佳的萃取条件,并应用于实际水样的测定。
2.采用了新型的液液扩散微萃取技术,将其和气相色谱串联质谱相结合,分析了水体中的氨基甲酸酯和有机磷农药残留,考察了影响液液扩散微萃取的条件,如萃取剂的类型和用量、扩散剂的类型和用量、萃取时间、pH值、离子强度,确定了最佳的条件,并将其应用于实际水样的测定,取得好的效果。
3.提出了微波辅助合成分子印迹固相萃取材料的方法,并将此材料应用于水样中克百威的分离富集,采紫外分光光度计法检测。优化了微波辅助悬浮聚合的合成条件,对克百威及其类似物进行了固相萃取吸附试验,并将该分子印迹固相材料应用于实际水样分析。
Carbamate and organophosphate pesticides were widely used to improve agricultural production. It's of great significance for improving the quantity and quality of agricultural products. Although these highly toxic pesticides can increase agricultural production and reduce the cost of lawn maintenance, etc., but the bioaccumulation of the food chain may affect human health. Traditional analysis methods of carbamate and organophosphorus pesticide residue such as liquid-liquid extraction, solid-phase extraction use large amounts of solvent, time-consuming, and it would cause secondary pollution to the environment. Therefore, an efficient, rapid method is required for the determination of carbamates and organic of pesticide residues.
In such cases, single drop liquid-liquid microextraction, liquid phase dispersive microextraction, molecularly imprinted solid-phase extraction is generated by a sample pretreatment technology. Single drop liquid-liquid phase microextraction mainly due to distribution of analytes between single drop of the syringe tip and the water samples; the liquid phase dispersive microextraction achieves a very large specific surface area and the mass transfer process can be completed in the shortest time; molecularly imprinted solid-phase extraction identifies with specific capabilities, and compared to traditional solid-phase extraction, can be reused. In this thesis, these three methods were used to determine the carbamate and organophosphate pesticide residues, respectively. The main research contents are as follows:
1. Single drop liquid-phase microextraction method was evaluated by analyzing carbamate and organophosphate pesticide residues at the same time. Gas chromatography mass spectrometry was used to analysis the water samples and investigated the impact of extraction of a variety of factors, such as the type and content of extractant, extraction time, pH, ionic strength, and to determine the best extraction conditions. The actual water samples was used analyzed in the conditions.
2. A new type of liquid phase dispersive microextraction was used coupled with gas chromatography tandem mass spectrometry to analysis water samples and carbamate pesticide residues. The impact of the dispersive of microextraction extraction conditions was investigated, such as the extractant type and content, the dispersive agents of the type and concentration, extraction time, pH, ionic strength. The best conditions was determined, and applied to the determination of the actual water samples.
3. Proposed a microwave-assisted synthesis of molecularly imprinted solid-phase extraction method, and carbofuran in water samples was used in the analysis under used of UV spectrophotometer analysis. The microwave-assisted synthesis conditions was optimized for suspension polymerization of carbofuran. Carbofuran and its analogues have done a solid-phase extraction assay, and the molecularly imprinted solid-phase materials used in practical analysis of water samples.
单滴液相微萃取、扩散微萃取、分子印迹固相萃取正是在这样情况下产生的新型样品前处理技术。单滴液相微萃取主要基于被分析物在微量进样器的针尖悬滴和水样体系之间的分配系数的不同;扩散微萃取的特点在于萃取溶剂充分扩散到水样中,获得极大的比表面积,使得被分析物能够在较短的时间内完成传质过程;分子印迹固相萃取具有特异的识别能力,并且相比于传统的固相萃取,能够重复使用。论文分别使用这三种先进的前处理技术,对氨基甲酸酯和有机磷农药残留前处理考察,主要研究内容有:
1.提出了单滴液相微萃取对氨基甲酸酯和有机磷农药残留同时测定的新方法,使用气相色谱质谱联用法分析,测定了水体中的氨基甲酸酯和有机磷农药残留。考察了影响萃取的各种因素,如萃取剂种类和用量、萃取时间、pH值、离子强度,最终确定了最佳的萃取条件,并应用于实际水样的测定。
2.采用了新型的液液扩散微萃取技术,将其和气相色谱串联质谱相结合,分析了水体中的氨基甲酸酯和有机磷农药残留,考察了影响液液扩散微萃取的条件,如萃取剂的类型和用量、扩散剂的类型和用量、萃取时间、pH值、离子强度,确定了最佳的条件,并将其应用于实际水样的测定,取得好的效果。
3.提出了微波辅助合成分子印迹固相萃取材料的方法,并将此材料应用于水样中克百威的分离富集,采紫外分光光度计法检测。优化了微波辅助悬浮聚合的合成条件,对克百威及其类似物进行了固相萃取吸附试验,并将该分子印迹固相材料应用于实际水样分析。
Carbamate and organophosphate pesticides were widely used to improve agricultural production. It's of great significance for improving the quantity and quality of agricultural products. Although these highly toxic pesticides can increase agricultural production and reduce the cost of lawn maintenance, etc., but the bioaccumulation of the food chain may affect human health. Traditional analysis methods of carbamate and organophosphorus pesticide residue such as liquid-liquid extraction, solid-phase extraction use large amounts of solvent, time-consuming, and it would cause secondary pollution to the environment. Therefore, an efficient, rapid method is required for the determination of carbamates and organic of pesticide residues.
In such cases, single drop liquid-liquid microextraction, liquid phase dispersive microextraction, molecularly imprinted solid-phase extraction is generated by a sample pretreatment technology. Single drop liquid-liquid phase microextraction mainly due to distribution of analytes between single drop of the syringe tip and the water samples; the liquid phase dispersive microextraction achieves a very large specific surface area and the mass transfer process can be completed in the shortest time; molecularly imprinted solid-phase extraction identifies with specific capabilities, and compared to traditional solid-phase extraction, can be reused. In this thesis, these three methods were used to determine the carbamate and organophosphate pesticide residues, respectively. The main research contents are as follows:
1. Single drop liquid-phase microextraction method was evaluated by analyzing carbamate and organophosphate pesticide residues at the same time. Gas chromatography mass spectrometry was used to analysis the water samples and investigated the impact of extraction of a variety of factors, such as the type and content of extractant, extraction time, pH, ionic strength, and to determine the best extraction conditions. The actual water samples was used analyzed in the conditions.
2. A new type of liquid phase dispersive microextraction was used coupled with gas chromatography tandem mass spectrometry to analysis water samples and carbamate pesticide residues. The impact of the dispersive of microextraction extraction conditions was investigated, such as the extractant type and content, the dispersive agents of the type and concentration, extraction time, pH, ionic strength. The best conditions was determined, and applied to the determination of the actual water samples.
3. Proposed a microwave-assisted synthesis of molecularly imprinted solid-phase extraction method, and carbofuran in water samples was used in the analysis under used of UV spectrophotometer analysis. The microwave-assisted synthesis conditions was optimized for suspension polymerization of carbofuran. Carbofuran and its analogues have done a solid-phase extraction assay, and the molecularly imprinted solid-phase materials used in practical analysis of water samples.
引文
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