钙黄绿素—钯荧光体系在农药残留检测中的应用研究
摘要
在农药的使用给农业带来巨大经济效益的同时也对环境与产品造成严重污染,为了更好地确保人们健康,必须加强对蔬菜水果中农药残留的监控。
农药残留常用的检测方法为色谱法,此外,还有免疫分析法、酶抑制法等快速检测方法。这些方法因各自所存在的缺点都不太适合于快速检测我国产销比较分散的果蔬等食品中的农药残留。相对而言,荧光光度法为农药提供了一条灵敏,价廉的测定途径,且荧光法无须昂贵仪器,操作简单。
鉴于此,本论文就着重研究了农药测定中的钙黄绿素-钯荧光光度法。具体开展的研究工作如下:
一.钙黄绿素-钯荧光体系研究
钙黄绿素是一种金属荧光试剂,它能与Pd2+发生配合反应,使其荧光猝灭。该部分系统研究了钙黄绿素的结构和性质,以及钙黄绿素和钙黄绿素-钯的荧光特性。
二.钙黄绿素-钯荧光体系在含硫有机磷农药残留检测中的应用研究
含硫有机磷农药能与Pd2+形成比钙黄绿素-钯更稳定的配合物,释放出钙黄绿素-钯配合物中的钙黄绿素,使溶液重显荧光,在一定浓度范围内,荧光强度与有机磷磷浓度呈线性关系。
1.钙黄绿素-钯荧光光度法在二硫代有机磷农药残留检测中的应用研究。系统研究了温度、酸度、反应时间、缓冲溶液用量等对钙黄绿素-钯荧光光度法测定二硫代有机磷农药甲拌磷的影响,建立了一种测定甲拌磷的新方法。该法的线性范围是2.0×10-8 ~ 2.0×10-7mol·L-1,相关系数r = 0.9988,检出限为5.3×10-9mol·L-1。用该法对土壤和甘蔗样品进行分析,并与色谱法对照,结果满意。
2.钙黄绿素-钯荧光光度法测定草莓中残留一硫代有机磷农药甲胺磷
以493 nm和514 nm为激发波长和发射波长,系统研究了反应条件对钙黄绿素-钯荧光光度法测定甲胺磷的影响,建立了一种测定甲胺磷的新方法。在40 oC,pH = 7.2的NaOH-KH2PO4缓冲溶液中,该法的线性范围是8.0×10-8 ~ 8.0×10-7 mol·L-1,相关系数r = 0.9963,检出限为1.42×10-8 mol·L-1。用该法对草莓样品进行分析,并与气相色谱法对照,结果一致。
3.钙黄绿素-钯荧光光度法测定青菜中残留一硫代有机磷农药氧乐果研究了钙黄绿素-钯荧光光度法测定氧乐果的方法。该方法的线性范围是8.0×10-8 ~ 8.0×10-7 mol·L-1,相关系数r = 0.9985,检出限为7.01×10-9 mol·L-1。该体系用于青菜中氧乐果农药残留测定,并进行了对照和回收率试验,取得了满意的结果。
Pesticide used in agriculture has greatly improved food production worldwide. However, due to the large scale application of organophosphorus pesticides, the residua of pesticides had brought serious environment pollution which became a greater and greater threaten to the health of human beings at present..Thus the analysis and determination of pesticide resdues in vegetables is very important.
Conventional methods for detecting residual pesticides included chromatography, innnunoassav analysis , biosensor and so on. However, the shortcomings of these methods their own, they were not suitable for determining the pesticide residues in fruits and vegetables for which production and distribution is scattered in our country. As a comparison, fluorophotometry provided a promising way to detect pesticides which was both sensitive and cheap. Furthermore, it is a simple method which does not need costly instruments.
So we placed emphasis on studying calcein - palladium fluorescence system applied in the detection of pesticide residues research and have done some work in this paper.
First. Study on calcein - palladium fluorescence system Calcein is a metal fluorescent reagent and it can form a complex with Pd 2+ to cause its fluorescence quenching. In this part, we study systematically the structure and properties of calcein and the fluorescence characteristics of calcein and calcein Pd 2+..
Second. The fluorometric determination of sulphur content organophosphorus pesticide residues with calcein Pd 2+
Sulphur content organophosphorus pesticide can form more stable complex with Pd2+ than calcein Pd2+, pesticide reacts with calcein Pd2+, the fluorescence of calein can be recovered. The change of fluorescence has a linear relationship with the concentration of pesticide .
1. The fluorometric determination of dithiocarbamate organic pesticide phorate pesticide residues with calcein Pd2+
A novel method to determine the trace phorate was proposed. The effects of temperature, solution acidity, reaction time, and quantities of buffer solution were examined on the determination of phorate with calcein Pd 2+ by fluorescence. The linear range is 2.0×10-8 ~2.0×10-7 mol·L-1 and the detection limit is 5.3×10-9 mol·L-1. The soil sample is analysed in this method and compared to the chromatogram measurement. The result is satisfied.
2. Calcein-Palladium fluorescence system applied in the detection of methamidophos in strawberry
Taking 493 nm and 514 nm as the excitation and emission wavelengths, respectively. The linear range is 2.0×10-8~2.0×10-7 mol·L-1 and the detection limit is 5.3×10-9 mol·L-1. Study Reaction conditions on the Calcein-Palladium Spectrophoto fluorimetry the impacting of methamidophos, and establish a new method of methamidophos determination. In the pH = 7.2 NaOH-KH2PO4 buffer solution and at 50℃, The linear range is 8.0×10-8 ~ 8.0×10-7 mol·L-1 and the detection limit is 1.42×10-8 mol·L-1, correlation coefficient is 0.9963. The strawberry is analysed in this method and compared to the chromatogram measurement. The result is satisfied.
3. Calcein-Palladium fluorescence system applied in the detection of Omethoate in vegetables
Study the method of Calcein-Palladium Spectrophotofluorimetry to determinate Omethoate. The linear range is 8.0×10-8 ~ 8.0×10-7 mol·L-1 and the detection limit is 7.9×10-9 mol·L-1.
农药残留常用的检测方法为色谱法,此外,还有免疫分析法、酶抑制法等快速检测方法。这些方法因各自所存在的缺点都不太适合于快速检测我国产销比较分散的果蔬等食品中的农药残留。相对而言,荧光光度法为农药提供了一条灵敏,价廉的测定途径,且荧光法无须昂贵仪器,操作简单。
鉴于此,本论文就着重研究了农药测定中的钙黄绿素-钯荧光光度法。具体开展的研究工作如下:
一.钙黄绿素-钯荧光体系研究
钙黄绿素是一种金属荧光试剂,它能与Pd2+发生配合反应,使其荧光猝灭。该部分系统研究了钙黄绿素的结构和性质,以及钙黄绿素和钙黄绿素-钯的荧光特性。
二.钙黄绿素-钯荧光体系在含硫有机磷农药残留检测中的应用研究
含硫有机磷农药能与Pd2+形成比钙黄绿素-钯更稳定的配合物,释放出钙黄绿素-钯配合物中的钙黄绿素,使溶液重显荧光,在一定浓度范围内,荧光强度与有机磷磷浓度呈线性关系。
1.钙黄绿素-钯荧光光度法在二硫代有机磷农药残留检测中的应用研究。系统研究了温度、酸度、反应时间、缓冲溶液用量等对钙黄绿素-钯荧光光度法测定二硫代有机磷农药甲拌磷的影响,建立了一种测定甲拌磷的新方法。该法的线性范围是2.0×10-8 ~ 2.0×10-7mol·L-1,相关系数r = 0.9988,检出限为5.3×10-9mol·L-1。用该法对土壤和甘蔗样品进行分析,并与色谱法对照,结果满意。
2.钙黄绿素-钯荧光光度法测定草莓中残留一硫代有机磷农药甲胺磷
以493 nm和514 nm为激发波长和发射波长,系统研究了反应条件对钙黄绿素-钯荧光光度法测定甲胺磷的影响,建立了一种测定甲胺磷的新方法。在40 oC,pH = 7.2的NaOH-KH2PO4缓冲溶液中,该法的线性范围是8.0×10-8 ~ 8.0×10-7 mol·L-1,相关系数r = 0.9963,检出限为1.42×10-8 mol·L-1。用该法对草莓样品进行分析,并与气相色谱法对照,结果一致。
3.钙黄绿素-钯荧光光度法测定青菜中残留一硫代有机磷农药氧乐果研究了钙黄绿素-钯荧光光度法测定氧乐果的方法。该方法的线性范围是8.0×10-8 ~ 8.0×10-7 mol·L-1,相关系数r = 0.9985,检出限为7.01×10-9 mol·L-1。该体系用于青菜中氧乐果农药残留测定,并进行了对照和回收率试验,取得了满意的结果。
Pesticide used in agriculture has greatly improved food production worldwide. However, due to the large scale application of organophosphorus pesticides, the residua of pesticides had brought serious environment pollution which became a greater and greater threaten to the health of human beings at present..Thus the analysis and determination of pesticide resdues in vegetables is very important.
Conventional methods for detecting residual pesticides included chromatography, innnunoassav analysis , biosensor and so on. However, the shortcomings of these methods their own, they were not suitable for determining the pesticide residues in fruits and vegetables for which production and distribution is scattered in our country. As a comparison, fluorophotometry provided a promising way to detect pesticides which was both sensitive and cheap. Furthermore, it is a simple method which does not need costly instruments.
So we placed emphasis on studying calcein - palladium fluorescence system applied in the detection of pesticide residues research and have done some work in this paper.
First. Study on calcein - palladium fluorescence system Calcein is a metal fluorescent reagent and it can form a complex with Pd 2+ to cause its fluorescence quenching. In this part, we study systematically the structure and properties of calcein and the fluorescence characteristics of calcein and calcein Pd 2+..
Second. The fluorometric determination of sulphur content organophosphorus pesticide residues with calcein Pd 2+
Sulphur content organophosphorus pesticide can form more stable complex with Pd2+ than calcein Pd2+, pesticide reacts with calcein Pd2+, the fluorescence of calein can be recovered. The change of fluorescence has a linear relationship with the concentration of pesticide .
1. The fluorometric determination of dithiocarbamate organic pesticide phorate pesticide residues with calcein Pd2+
A novel method to determine the trace phorate was proposed. The effects of temperature, solution acidity, reaction time, and quantities of buffer solution were examined on the determination of phorate with calcein Pd 2+ by fluorescence. The linear range is 2.0×10-8 ~2.0×10-7 mol·L-1 and the detection limit is 5.3×10-9 mol·L-1. The soil sample is analysed in this method and compared to the chromatogram measurement. The result is satisfied.
2. Calcein-Palladium fluorescence system applied in the detection of methamidophos in strawberry
Taking 493 nm and 514 nm as the excitation and emission wavelengths, respectively. The linear range is 2.0×10-8~2.0×10-7 mol·L-1 and the detection limit is 5.3×10-9 mol·L-1. Study Reaction conditions on the Calcein-Palladium Spectrophoto fluorimetry the impacting of methamidophos, and establish a new method of methamidophos determination. In the pH = 7.2 NaOH-KH2PO4 buffer solution and at 50℃, The linear range is 8.0×10-8 ~ 8.0×10-7 mol·L-1 and the detection limit is 1.42×10-8 mol·L-1, correlation coefficient is 0.9963. The strawberry is analysed in this method and compared to the chromatogram measurement. The result is satisfied.
3. Calcein-Palladium fluorescence system applied in the detection of Omethoate in vegetables
Study the method of Calcein-Palladium Spectrophotofluorimetry to determinate Omethoate. The linear range is 8.0×10-8 ~ 8.0×10-7 mol·L-1 and the detection limit is 7.9×10-9 mol·L-1.
引文
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