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机构地区:[1]南昌大学食品科学与技术国家重点实验室,江西南昌330047 [2]南昌大学化学系,江西南昌330031
出 处:《分析科学学报》2012年第6期747-751,共5页Journal of Analytical Science
基 金:国家自然科学基金(No.21065007);南昌大学食品科学与技术国家重点实验室基金(No.SKLF-MB-200807;SKLF-TS-200919)
摘 要:本文采用动力学分光光度法结合化学计量学方法对水样中的两种氨基甲酸酯类农药杀线威和抗蚜威进行测定。该方法基于酸性条件下,Cu(Ⅱ)能催化H2O2氧化罗丹明B而使其褪色,杀线威或抗蚜威存在时能使该反应速率降低,而且两者对反应速率的影响存在一定差异。实验对硫酸浓度、Cu(Ⅱ)浓度、罗丹明B浓度、H2O2的质量分数以及温度等条件进行考察。在选定实验条件下,杀线威和抗蚜威测定的线性范围分别为2~16μg.mL-1和1~15μg.mL-1,检测限分别为0.65μg.mL-1和0.41μg.mL-1。实验采集波长554nm处和反应时间0~600s范围内动力学吸光度数据,并分别采用偏最小二乘法(PLS)和主成分回归法(PCR)处理,建立了定量回归模型并对合成样品进行测定以验证模型。该方法可应用于实际水样中杀线威和抗蚜威的同时测定。In this paper, a kinetic spectrophotometric method was developed for simultaneous determination of oxamyl and pirimicarb,with the application of partial least square(PLS) and principal component regression(PCR) to resolve the overlapping spectral kinetic data. The method was based on the inhibitory effect of oxamyl and pirimicarb on the Cu( II ) catalyzed oxidation of rhodamine B by hydrogen peroxide in sulfuric acid. The effect of different parameters, such as concentration of reactants and temperature on the rate of reaction, was investigated. Under the optimum conditions, the linear ranges for determination of oxamyl and pirimicarb were 2-16 ug · mL- 1 and 1-15 ug· mL- 1 , respectively, and the corresponding detection limits for oxamyl and pirimicarb were 0.65 ug · mL -1 and 0.41 ug·mL- 1, respectively. The proposed method was applied to the simultaneous determination of oxamyl and pirimicarb in two spiked water samples,obtaining satisfactory results with recoveries of 93.2 %-103.1 %.
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