| HPLC分析土壤中辛硫磷的前处理方法研究 |
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| 引用本文： | 杨秀群,余 磊,张桂玲,严学芬,赵 杰.HPLC分析土壤中辛硫磷的前处理方法研究[J].贵阳金筑大学学报,2013(4):12-16. |
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| 作者姓名： | 杨秀群 余 磊 张桂玲 严学芬 赵 杰 |
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| 作者单位： | [1]贵阳学院教学设备及实验管理中心,贵州贵阳550005 [2]贵阳学院化学与材料工程学院,贵州贵阳550005 |
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| 基金项目： | 贵阳学院院级科研项目“辛硫磷在液相色谱和气相色谱分析中前处理方法的对比研究”（项目编号：201117）阶段性成果. |
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| 摘 要： | 建立了HPLC检测土壤中辛硫磷的前处理方法,考察了提取溶剂种类,提取时间和溶剂用量.最佳实验条件为：用60mL乙酸乙酯作萃取溶剂,振荡提取50 min,经旋转蒸发仪浓缩,甲醇定容至5mL,过滤.滤液于高效液相色谱仪-二极管阵列检测器检测,用C18色谱柱,进样量10uL,流动相为V（乙腈）：V（水）=7：3,检测波长为283nm.辛硫磷在0.6～30.00μg/mL之间有良好的线性关系,相关系数为0.9999,加标回收率达88.27％,精密度（n=6）为3.35％.该方法具有较高的灵敏度和准确性.
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| 关 键 词： | 前处理方法 辛硫磷 高效液相色谱法 振荡萃取 |
Pretreatment methods for the Determination of analysis of Phoxim in Soil by HPLC |
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| YANG Xiu-qun,YU lei,ZHANG Gui-ling,YAN Xue-fen,ZHAO Jie.Pretreatment methods for the Determination of analysis of Phoxim in Soil by HPLC[J].Journal of Jinzhu University of Guiyang,2013(4):12-16. |
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| Authors: | YANG Xiu-qun YU lei ZHANG Gui-ling YAN Xue-fen ZHAO Jie |
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| Institution: | 1. Experimental equipment and teaching management center of Guiyang College, Guiyang , Guizhou550005 ; 2. Chemical and Materials Engineering of Guiyang College, Guiyang , Guizhou550005 ) |
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| Abstract: | A pretreatment method for the determination of Phoxim in siol by HPLC was established. The extraction sol- vent types, extraction time and solvent volume was investigated. The optimum experimental conditions was this： Used 60mL ethyl acetate as the extraction solvent, shaking extraction 50min, solvent had been concentrated by rotary evapora- tor then be volumed to 5mL With methanol, filtered last. The sample was detected by HPLC with DAD detector. Used C18 column, the Injection volume was 101~L, solvent ratio was V （acetonitrile） ： V （water） = 7 ： 3, detection wave- length of 283nm. The linearity of phoxim were good between 0.61xg/mL and 30txg/mL, the RWas 0. 9999, the recovery rate of Phoxim was to 88.27%. The coefficient of variation was 3.35% which made 6 times repeated tests. The new method was high sensitivity and accuracy. |
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| Keywords: | Pretreatment Phoxim HPLC Oscillation extraction |
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