快速溶剂萃取·固相萃取净化·超高效液相色谱法在土壤农药残留测定中的应用 |
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引用本文: | 张永兵,杨文武,丁金美,何娟. 快速溶剂萃取·固相萃取净化·超高效液相色谱法在土壤农药残留测定中的应用[J]. 安徽农业科学, 2013, 0(33): 12870-12871,12873 |
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作者姓名: | 张永兵 杨文武 丁金美 何娟 |
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作者单位: | 泰州市环境监测中心站,江苏省环境保护土壤有机污染物监测重点实验室,江苏泰州225300;泰州市环境监测中心站,江苏省环境保护土壤有机污染物监测重点实验室,江苏泰州225300;泰州市环境监测中心站,江苏省环境保护土壤有机污染物监测重点实验室,江苏泰州225300;泰州市环境监测中心站,江苏省环境保护土壤有机污染物监测重点实验室,江苏泰州225300 |
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基金项目: | 863项目(2013AA06A309). |
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摘 要: | [目的]建立土壤中灭草松、莠去津和2,-4滴的快速分析方法。[方法]建立了快速溶剂萃取一固相萃取净化一超高效液相色谱法测定土壤中的灭草松、莠去津和2,-4滴农药。[结果]优化了快速溶剂萃取条件,影响快速溶剂萃取的4种因子显著性为溶剂类型〉溶剂体积〉静态萃取时间〉提取温度。最佳快速溶剂萃取条件:温度=120℃,M土壤/V提取溶剂=1:3,溶剂为乙腈,静态萃取时间为15min。检出限为0.01~0.05mg/kg,加标回收率在76.4%-91.3%,相对标准偏差RSD〈10%(n=7)。[结论]该法操作方便,灵敏度高,可用于土壤中灭草松、莠去津和2,4.滴的测定。
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关 键 词: | 灭草松 莠去津 2 -4滴 快速溶剂萃取 超高效液相色谱 土壤 |
Application of ASE-SPE-UPLC Method in Soil Pesticide Residues Determination |
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Affiliation: | ZHANG Yong-bing et ai ( Environmental Monitor Center of Taizhou, Taizhou; Jiangsu 225300) |
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Abstract: | [ Objective] To establish a rapid analysis method for Bentazone, Atrazine and 2,4-D in soil. [ Method] A method for the determination of Bentazone, Atrazine and 2,4-D in soil was established which is extiacted by ASE, purified by SPE and determined by UPLC. [ Result ] Optimization is conducted for the four main factors ( extracting temperature, soil weight/volume of extracting solvent, extracting solvent, extracting time) that Would affect recovery rate by orthogonal test. The order of influence on ASE is extracting solvent 〉 soil weight/volume of extracting solvent 〉 extracting time 〉 extracting temperature. Optimal results are determined as follows : T = 120 %, soil weight/volume of extracting solvent is 1/3, extracting solvent is acetonitrile, extracting time is 15 min. The limits of quantification for all Bentazone, Atrazine and 2,4-D are 0.01 - 0.05 mg/kg in about 10.00 g soil samples. The RSD 〈 10% ( n = 7 ) and the recoveries are between 76.4% - 91.3%. [ Conclusion] The results show that this method is sensitive, simple and suitable for the determination of Bentazone, Atrazine and 2, 4-D in soil. |
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Keywords: | Bentazone Atrazine 2,4-D Accelerated solvent extraction Rapid UPLC Soil |
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