浊点萃取的农药残留分析方法研究和甲醛的快速检测
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摘要
近年来，农产品、饮用水、环境中有关于农药残留的问题越来越引起人们的重视，为了保护人们的身体健康，WHO／FAO-CAC对食品中农药残留作了相应的最高残留限量(MRL)的规定。开发一种针对我国食品中农兽药残留问题和国际食品贸易要求的简单、快速、有效的样品前处理技术以及具有高灵敏度和高选择性的多残留检测技术就显得十分重要。人们对居住环境和食品的安全问题也同样重视，特别是甲醛的污染，为此研究甲醛的快速检测很有实用价值。
本论文共分三个部分：
第一部分：浊点萃取在高效液相色谱检测牛奶中6种农药的应用
建立应用浊点萃取法对牛奶中的残留除草剂进行萃取富集后用高效液相色谱(HPLC)检测的方法。以6％的表面活性剂Tween20或Triton X-100为萃取剂，在一定浓度的(NH_4)_2SO_4或NaCl的存在下加热萃取。牛奶中6种不同的除草剂被胶束相富集后被HPLC分离检测，结果表明：肟草酮、嗪草酮和溴苯腈在20-10000ng／ml，苯噻草胺在30-10000 ng／ml，苄嘧磺隆和烟嘧磺隆在50-10000 ng／ml和检测信号呈线性，相关系数为0.9981-0.9997，平均加标回收率在85.09-96.74％之间，相对标准偏差为1.90％-3.98％。试验的6种农药测得的定量检测限均小于国家规定的农药残留限量(MRL)。该方法简便、快速、灵敏、污染少，实际应用性好。
第二部分：涂料中甲醛的分光光度测定新方法
在FeCl_3存在的盐酸介质中，甲醛与蛋白胨反应生成紫色化合物，最大吸收波长555nm，甲醛浓度在1-25μg／10mL范围内，吸光度与浓度成线性关系，线性相关系数是r~2=0.9997，检出限0.05μg／mL。用本法测定经活性炭脱色的水溶性涂料中的甲醛含量，回收率为96.46-103.32％，相对标准偏差为1.36-2.09％(n=6)。
第三部分：酒类中微量甲醛的快速测定新方法
在FeCl_3存在条件下，甲醛与自制蛋白液显色剂能产生紫色化合物，可以定量测定微量甲醛。定量测定范围1-10μg／10ml，线性相关系数是r~2=0.996，最低检出限0.05μg／ml。用该法测定经活性炭脱色的啤酒和白酒中的甲醛含量，回收率为96.46-103.32％，相对标准偏差为1.36-2.09％(n=6)。
Residue of pesticides found in agriculture products, drinking water and environmental exposure has raised much concern from the general public in recent years. In order to protect persons' healthy, the maximum residue levels (MRL) in food were constituted by WHO/FAO-CAC. It is important to exploit simply, fast, efficient pre-treatment technologies for samples and high sensitive, high selective multi-pesticide detections technologies based on pesticide and veterinary drug residues in food and the requirement for international trade on food. The safty of the living environment and foods also cause people attention especially about formaldehyde pollution. The study of formaldehyde instant determination become valuable.
The thesis includes three parts:
In chapterⅠ: The application of cloud point extraction in determination 6 types pesticides in milk by HPLC
The feasibility of employing cloud point extraction (CPE) as extraction and preconcentration method for recovery of herbicide from milk samples followed by HPLC analysis is demonstrated. An aqueous surfactant solution containing 6% Tween20 or Triton X-100 was used and then heated with appropriate concentration (NH_4)_2SO_4 or NaCl for extraction of herbicide. The extraction was analyzed by HPLC in next step. Six herbicides in milk were analyzed simultaneous. Results show linear dynamic range of detection of Tralkoxydim、Metribuzin and Bormoxynil were 20-10000 ng/ml, Mefenacet was 20-10000 ng/ml, Bensulfuron-Methyl and Nicosulfuron were 20-10000 ng/ml. The correlation coefficient were 0.9981～0.9997. The average recoveries of the six herbicides ranged from 85.09% to 96.74%. The relative standard deviations for the six herbicides were in the range of 1.90%～3.98%. The limit of detection about 6 type's pesticides is lower than GB MRL. The results indicate that the method developed is easier, faster, sensitive and less pollution. It can be used for analyses the other things.
In chapterⅡ: A new spectrophotometry method for instant determination of formaldehyde in dope
In the presence of FeCl_3 and HCl, formaldehyde can form a purple complex with peptone The complex exhibited max absorption at 555nm. The absorption was linearly proportional to the complex concentration in the formaldehyde concentration range of 1～25μg/10mL, a correlation coefficient (r~2) was 0.9997. The detection limit was 0.05μg/mL. This method was applied to the determination of formaldehyde in dope discoloring by the active carbon. And the recoveries were 96.46—103.32%, the relative standard deviations were 1.36—2.09% (n=6).
In chapterⅢ: A new method for instant determination of trace formaldehyde in alcohol
A new method for determination of trace formaldehyde in beer was developed by a spectrophotometer at 555nm. Based on studies of reaction conditions, e. g. reagent concentration, reaction temperature and time, a colorimetric method was established. A 4ml volume of egg white reagent and a 1.0ml volume of FeCl_3 solution were added into a 4ml volume of a beer sample, and the mixture was heated at 70℃for 10 min. After cooling, the coloring solution was determined. The detection limits were 1～10μg/10ml in beer, a correlation coefficient (r~2) was 0.996. The recoveries were 96.46—103.32% and relative standard deviations were 1.36—2.09% (n=6).
本论文共分三个部分：
第一部分：浊点萃取在高效液相色谱检测牛奶中6种农药的应用
建立应用浊点萃取法对牛奶中的残留除草剂进行萃取富集后用高效液相色谱(HPLC)检测的方法。以6％的表面活性剂Tween20或Triton X-100为萃取剂，在一定浓度的(NH_4)_2SO_4或NaCl的存在下加热萃取。牛奶中6种不同的除草剂被胶束相富集后被HPLC分离检测，结果表明：肟草酮、嗪草酮和溴苯腈在20-10000ng／ml，苯噻草胺在30-10000 ng／ml，苄嘧磺隆和烟嘧磺隆在50-10000 ng／ml和检测信号呈线性，相关系数为0.9981-0.9997，平均加标回收率在85.09-96.74％之间，相对标准偏差为1.90％-3.98％。试验的6种农药测得的定量检测限均小于国家规定的农药残留限量(MRL)。该方法简便、快速、灵敏、污染少，实际应用性好。
第二部分：涂料中甲醛的分光光度测定新方法
在FeCl_3存在的盐酸介质中，甲醛与蛋白胨反应生成紫色化合物，最大吸收波长555nm，甲醛浓度在1-25μg／10mL范围内，吸光度与浓度成线性关系，线性相关系数是r~2=0.9997，检出限0.05μg／mL。用本法测定经活性炭脱色的水溶性涂料中的甲醛含量，回收率为96.46-103.32％，相对标准偏差为1.36-2.09％(n=6)。
第三部分：酒类中微量甲醛的快速测定新方法
在FeCl_3存在条件下，甲醛与自制蛋白液显色剂能产生紫色化合物，可以定量测定微量甲醛。定量测定范围1-10μg／10ml，线性相关系数是r~2=0.996，最低检出限0.05μg／ml。用该法测定经活性炭脱色的啤酒和白酒中的甲醛含量，回收率为96.46-103.32％，相对标准偏差为1.36-2.09％(n=6)。
Residue of pesticides found in agriculture products, drinking water and environmental exposure has raised much concern from the general public in recent years. In order to protect persons' healthy, the maximum residue levels (MRL) in food were constituted by WHO/FAO-CAC. It is important to exploit simply, fast, efficient pre-treatment technologies for samples and high sensitive, high selective multi-pesticide detections technologies based on pesticide and veterinary drug residues in food and the requirement for international trade on food. The safty of the living environment and foods also cause people attention especially about formaldehyde pollution. The study of formaldehyde instant determination become valuable.
The thesis includes three parts:
In chapterⅠ: The application of cloud point extraction in determination 6 types pesticides in milk by HPLC
The feasibility of employing cloud point extraction (CPE) as extraction and preconcentration method for recovery of herbicide from milk samples followed by HPLC analysis is demonstrated. An aqueous surfactant solution containing 6% Tween20 or Triton X-100 was used and then heated with appropriate concentration (NH_4)_2SO_4 or NaCl for extraction of herbicide. The extraction was analyzed by HPLC in next step. Six herbicides in milk were analyzed simultaneous. Results show linear dynamic range of detection of Tralkoxydim、Metribuzin and Bormoxynil were 20-10000 ng/ml, Mefenacet was 20-10000 ng/ml, Bensulfuron-Methyl and Nicosulfuron were 20-10000 ng/ml. The correlation coefficient were 0.9981～0.9997. The average recoveries of the six herbicides ranged from 85.09% to 96.74%. The relative standard deviations for the six herbicides were in the range of 1.90%～3.98%. The limit of detection about 6 type's pesticides is lower than GB MRL. The results indicate that the method developed is easier, faster, sensitive and less pollution. It can be used for analyses the other things.
In chapterⅡ: A new spectrophotometry method for instant determination of formaldehyde in dope
In the presence of FeCl_3 and HCl, formaldehyde can form a purple complex with peptone The complex exhibited max absorption at 555nm. The absorption was linearly proportional to the complex concentration in the formaldehyde concentration range of 1～25μg/10mL, a correlation coefficient (r~2) was 0.9997. The detection limit was 0.05μg/mL. This method was applied to the determination of formaldehyde in dope discoloring by the active carbon. And the recoveries were 96.46—103.32%, the relative standard deviations were 1.36—2.09% (n=6).
In chapterⅢ: A new method for instant determination of trace formaldehyde in alcohol
A new method for determination of trace formaldehyde in beer was developed by a spectrophotometer at 555nm. Based on studies of reaction conditions, e. g. reagent concentration, reaction temperature and time, a colorimetric method was established. A 4ml volume of egg white reagent and a 1.0ml volume of FeCl_3 solution were added into a 4ml volume of a beer sample, and the mixture was heated at 70℃for 10 min. After cooling, the coloring solution was determined. The detection limits were 1～10μg/10ml in beer, a correlation coefficient (r~2) was 0.996. The recoveries were 96.46—103.32% and relative standard deviations were 1.36—2.09% (n=6).
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