阿维菌素和高氯在甘蓝和土壤中的残留消解动态及阿维菌素的光解研究
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摘要
本文首先建立了阿维菌素和高效氯氰菊酯在土壤和甘蓝中的残留分析方法,在此基础上,研究了阿维菌素和高效氯氰菊酯在土壤和甘蓝中的残留消解动态和最终残留量,并利用人工光源研究了阿维菌素在水溶液中的光化学降解规律。
甘蓝中阿维菌素用乙酸乙酯提取,浓缩干后用乙腈溶解定容。土壤中阿维菌素用水和乙腈提取,浓缩干后用乙腈溶解定容。样品经衍生化后用HPLC(FLD)测定。阿维菌素的最小检测量为0.1ng,甘蓝和土壤样品中阿维菌素最小检测浓度为0.002mg/kg。添加浓度0.005-0.5mg/kg时,土壤中回收率可达77.74-90.32%,变异系数1.50-4.78%;甘蓝中回收率可达75.68-84.52%,变异系数1.98-3.18%,符合农药残留分析要求。
甘蓝中高氯用乙腈提取;土壤中高氯用水和乙腈提取,后分别用弗罗里硅土柱层析净化,浓缩干后用正己烷溶解定容。样品用气相色谱(ECD)测定。高氯的最小检测量为0.01ng,甘蓝和土壤样品中高氯的最小检测浓度为0.01mg/kg。添加浓度0.01-1mg/kg时,土壤中回收率可达86.37-104.66%,变异系数3.51-4.53%;甘蓝中回收率可达96.55-114.86%,变异系数2.96-6.61%;符合农药残留分析要求。
采用上述方法,测定了2007年和2008年2.4%阿维·高氯微乳剂在安徽和北京两地甘蓝和土壤中的消解动态及最终残留量。结果表明,07年阿维菌素在安徽土壤中的降解半衰期为1.98天;在甘蓝上的降解半衰期为2天;08年在安徽和北京两地的土壤中的降解半衰期分别为1.06天、1.55天;在甘蓝上的降解半衰期分别为0.94天、1.14天。07年高氯在安徽土壤中的降解半衰期为3.28天;在甘蓝上的降解半衰期为3.77天;08年在安徽和北京两地的土壤中的降解半衰期分别为7.52天、10.98天;在甘蓝上的降解半衰期分别为4.73天、3.07天。2.4%阿维·高氯微乳剂在安徽和北京两地施用后,甘蓝和土壤中阿维菌素的最终残留量均小于LOQ;高氯只在甘蓝中有少量残留,且均低于我国和日本关于氯氰菊酯在甘蓝中的残留限量标准(分别为2.0和1.0 mg/kg)。
阿维菌素在水溶液中的光解均呈一级动力学反应。阿维菌素在紫外灯下的光解速率比高压汞灯下快;阿维菌素光解速率随其初始浓度增大而减小,随pH增大而增大;硝酸盐、十二烷基磺酸钠、色素等水中共存污染物对阿维菌素的光解均有光猝灭效应,且硝酸盐和十二烷基磺酸钠对阿维菌素的光猝灭作用随添加浓度的增大而增强。
Residues analytical methods of Avermectin and Beta-Cypermethrin in cabbage and soil were established. Dissipation and the terminal residues of Avermectin and Beta-Cypermethrin in cabbage and soil, as well as photochemical degradation of Avermectin in aqueous solution, were studied in this paper.
Residues of Avermectin were extracted from cabbage with acetic ether, while residues of Avermectin were extracted from soil with acetonitrile and water, and determined by HPLC(FLD). The limit of detection of Avermectin (LOD) was 0.1ng and the method detection limit (MDL)of Avermectin in the samples of cabbage and soil was 0.002mg/kg.The average recoveries and coefficient of variations of the method were 77.74 ~ 90.32%,1.50-4.78% for soil samples ,and 75.68 ~ 84.52%, 1.98-3.18% for cabbage samples, respectively. These results showed that the method accords with demands of residue analysis of pesticides.
Residues of Beta-Cypermethrin were extracted from cabbage with acetonitrile, while residues of Beta-Cypermethrin were extracted from soil with acetonitrile and water, cleaned up with florsil and determined by GC-ECD. The limit of detection of Beta-Cypermethrin (LOD) was 0.01ng and the method detection limit (MDL) of Beta-Cypermethrin in the samples of cabbage and soil was 0.01mg/kg.The average recoveries and coefficient of variations of the method were 86.37~104.66%,3.51~ 4.53% for soil samples ,and 96.55~114.86%, 2.96~6.61% for cabbage samples, respectively. These results showed that the method accords with demands of residue analysis of pesticide.
With the mentioned method, dissipation dynamics and the terminal residues of Avermectin and Beta-Cypermethrin in cabbage and soil had been studied in Anhui and Beijing during 2007 and 2008.The results showed that the dissipation halflife of Avermectin in soil in Anhui in 2007 was 1.98 d ; the dissipation halflife in cabbage was 2d ; the dissipation halflives of Avermectin in soil in Anhui and Beijing in 2008 were 1.06d,1.55d, respectively ; the dissipation halflives in cabbage were 0.94d,1.14d, respectively ; the dissipation halflife of Beta-Cypermethrin in soil in Anhui in 2007 was 3.28d; the dissipation halflife in cabbage was 3.77d; the dissipation halflife of Beta-Cypermethrin in soil in Anhui and Beijing in 2008 were 7.52d, 10.98d, respectively.; the dissipation halflives in cabbage were 4.73d、3.07d, respectively. The terminal residues of avermectin in both cabbage and soil were less than LOQ ; The terminal residues of Beta-Cypermethrin in cabbage were lower than the MRL in china and Japan (2.0 and 1.0 mg / kg , respectively).
Photochemical degradation of Avermectin in aqueous solution followed the first order reaction. The results showed that the photodegradation rate of Avermectin under UV lamp irradiation was quicker than under high pressure mercury lamp(HPML) irradiation. The photolytic degradation rate of Avermectin decreased with the initial concentrations increasing and with the pH value decreasing. SDS、nitrate and pigments exhibited photoquenching effects on the photolysis of Avermectin, the photoquenching effects increased with the concentrations increasing of SDS and nitrate.
甘蓝中阿维菌素用乙酸乙酯提取,浓缩干后用乙腈溶解定容。土壤中阿维菌素用水和乙腈提取,浓缩干后用乙腈溶解定容。样品经衍生化后用HPLC(FLD)测定。阿维菌素的最小检测量为0.1ng,甘蓝和土壤样品中阿维菌素最小检测浓度为0.002mg/kg。添加浓度0.005-0.5mg/kg时,土壤中回收率可达77.74-90.32%,变异系数1.50-4.78%;甘蓝中回收率可达75.68-84.52%,变异系数1.98-3.18%,符合农药残留分析要求。
甘蓝中高氯用乙腈提取;土壤中高氯用水和乙腈提取,后分别用弗罗里硅土柱层析净化,浓缩干后用正己烷溶解定容。样品用气相色谱(ECD)测定。高氯的最小检测量为0.01ng,甘蓝和土壤样品中高氯的最小检测浓度为0.01mg/kg。添加浓度0.01-1mg/kg时,土壤中回收率可达86.37-104.66%,变异系数3.51-4.53%;甘蓝中回收率可达96.55-114.86%,变异系数2.96-6.61%;符合农药残留分析要求。
采用上述方法,测定了2007年和2008年2.4%阿维·高氯微乳剂在安徽和北京两地甘蓝和土壤中的消解动态及最终残留量。结果表明,07年阿维菌素在安徽土壤中的降解半衰期为1.98天;在甘蓝上的降解半衰期为2天;08年在安徽和北京两地的土壤中的降解半衰期分别为1.06天、1.55天;在甘蓝上的降解半衰期分别为0.94天、1.14天。07年高氯在安徽土壤中的降解半衰期为3.28天;在甘蓝上的降解半衰期为3.77天;08年在安徽和北京两地的土壤中的降解半衰期分别为7.52天、10.98天;在甘蓝上的降解半衰期分别为4.73天、3.07天。2.4%阿维·高氯微乳剂在安徽和北京两地施用后,甘蓝和土壤中阿维菌素的最终残留量均小于LOQ;高氯只在甘蓝中有少量残留,且均低于我国和日本关于氯氰菊酯在甘蓝中的残留限量标准(分别为2.0和1.0 mg/kg)。
阿维菌素在水溶液中的光解均呈一级动力学反应。阿维菌素在紫外灯下的光解速率比高压汞灯下快;阿维菌素光解速率随其初始浓度增大而减小,随pH增大而增大;硝酸盐、十二烷基磺酸钠、色素等水中共存污染物对阿维菌素的光解均有光猝灭效应,且硝酸盐和十二烷基磺酸钠对阿维菌素的光猝灭作用随添加浓度的增大而增强。
Residues analytical methods of Avermectin and Beta-Cypermethrin in cabbage and soil were established. Dissipation and the terminal residues of Avermectin and Beta-Cypermethrin in cabbage and soil, as well as photochemical degradation of Avermectin in aqueous solution, were studied in this paper.
Residues of Avermectin were extracted from cabbage with acetic ether, while residues of Avermectin were extracted from soil with acetonitrile and water, and determined by HPLC(FLD). The limit of detection of Avermectin (LOD) was 0.1ng and the method detection limit (MDL)of Avermectin in the samples of cabbage and soil was 0.002mg/kg.The average recoveries and coefficient of variations of the method were 77.74 ~ 90.32%,1.50-4.78% for soil samples ,and 75.68 ~ 84.52%, 1.98-3.18% for cabbage samples, respectively. These results showed that the method accords with demands of residue analysis of pesticides.
Residues of Beta-Cypermethrin were extracted from cabbage with acetonitrile, while residues of Beta-Cypermethrin were extracted from soil with acetonitrile and water, cleaned up with florsil and determined by GC-ECD. The limit of detection of Beta-Cypermethrin (LOD) was 0.01ng and the method detection limit (MDL) of Beta-Cypermethrin in the samples of cabbage and soil was 0.01mg/kg.The average recoveries and coefficient of variations of the method were 86.37~104.66%,3.51~ 4.53% for soil samples ,and 96.55~114.86%, 2.96~6.61% for cabbage samples, respectively. These results showed that the method accords with demands of residue analysis of pesticide.
With the mentioned method, dissipation dynamics and the terminal residues of Avermectin and Beta-Cypermethrin in cabbage and soil had been studied in Anhui and Beijing during 2007 and 2008.The results showed that the dissipation halflife of Avermectin in soil in Anhui in 2007 was 1.98 d ; the dissipation halflife in cabbage was 2d ; the dissipation halflives of Avermectin in soil in Anhui and Beijing in 2008 were 1.06d,1.55d, respectively ; the dissipation halflives in cabbage were 0.94d,1.14d, respectively ; the dissipation halflife of Beta-Cypermethrin in soil in Anhui in 2007 was 3.28d; the dissipation halflife in cabbage was 3.77d; the dissipation halflife of Beta-Cypermethrin in soil in Anhui and Beijing in 2008 were 7.52d, 10.98d, respectively.; the dissipation halflives in cabbage were 4.73d、3.07d, respectively. The terminal residues of avermectin in both cabbage and soil were less than LOQ ; The terminal residues of Beta-Cypermethrin in cabbage were lower than the MRL in china and Japan (2.0 and 1.0 mg / kg , respectively).
Photochemical degradation of Avermectin in aqueous solution followed the first order reaction. The results showed that the photodegradation rate of Avermectin under UV lamp irradiation was quicker than under high pressure mercury lamp(HPML) irradiation. The photolytic degradation rate of Avermectin decreased with the initial concentrations increasing and with the pH value decreasing. SDS、nitrate and pigments exhibited photoquenching effects on the photolysis of Avermectin, the photoquenching effects increased with the concentrations increasing of SDS and nitrate.
引文
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