摘要
采用Kromasil C18不锈钢柱（250mm×4．6mm i．d.，5μm），以V（甲醇）：V（水）=70：30混合溶剂为流动相（pH用H3PO4调至3.0），流速1．0mL／min，检测波长236nm和柱温35℃，建立了不同水体中甲硫嘧磺隆残留的样品处理方法和高效液相色谱分析方法。甲硫嘧磺隆在0．25～10mg／L范围内，其峰面积（U）与质量浓度（ρ）呈现良好的相关性，其线性回归方程为Y=4425．9ρ＋5664．8，R^2=0．9997。在纯净水、池塘水、河水、稻田水A和稻田水B中，甲硫嘧磺隆5个添加浓度水平的平均回收率分别为92．80％～101．53％、92．54％～103．10％％、94．11％～97．57％、92．91％～101．25％和84．94％～92．53％．RsD分别为0．43％～4．1％、0．85％～6．5％、0．37％～7．0％、0．56％～7．7％和1．4％～4．7％，检出限（LOD）为1．50×10^-9 g（S／N=3）。可用于环境水样中甲硫嘧磺隆的残留量检测。
A quantitative high performance liquid chromatographic method using diode array detector has been developed for the determination of novel sulfonylurea herbicide methiopyrsulfuron [ methyl 2-（4-methoxyl-6-methylthio-2-pyrimidinyl） aminocarbonyl sulfonyl benzoate, MPS] residues in the environmental aquatic systems. MPS was extracted by liquid-liquid partition from water samples （which were adjusted to pH 3.0 with 5% sulfuric acid） into dichloromethane. A Kromasil C18 stainless steel column （250 mm×4.6 mm i.d., 5μm） was used with mixture of methanol-water （70：30, V/V） as the mobile phase （pH adjusted to 3.0） at a flow rate of 1.0 mL/min. The column tem- perature was 35℃, and the ultraviolet detection wavelength was 236 nm. The calibration curve for MPS was in good linearity in the concentration range of 0.25 - 10 mg/L with the regression equation Y = 4425.9ρ ＋ 5664.8, R^2 = 0.9997. The average recoveries of five spiked concentration levels for MPS in pure water, pond water, river water, paddy field water A and B were 92.80% - 101.53 %, 92,54 % - 103.10% %, 94.11% - 97.57 %, 92.91% 101.25% and 84.94% - 92.53%, respectively. The coefficients of variation （CV） were 0.43% - 4.12%, 85% 6.47%, 0.37% - 6.96%, 0.56% - 7.70% and 1.37% - 4.70%, respectively. The limit of detection （LOD） for MPS was 1.50×l0^-9 g （S/N = 3）. The results indicate that the method is fast, sensitive, reproducible and practical for the residue detection and analysis of MPS in aquatic systems.
出处
《分析试验室》
CAS
CSCD
北大核心
2008年第8期13-16,共4页
Chinese Journal of Analysis Laboratory
基金
国家十一五科技支撑计划(2006BAE01A04-4)项目资助
