基质固相分散-高效液相色谱法测定鲫鱼肌肉中残留的辛硫磷  

Application of matrix solid-phase dispersion for the determination of phoxim in crucian carp samples by high performance liquid chromatography

作　　者：刘茜[1] 刘晓宇[1] 邱朝坤[1] 王小宝[1] 任红敏[1] 

机构地区：[1]华中农业大学食品科技学院,湖北武汉430070

出　　处：《色谱》2009年第4期476-479,共4页Chinese Journal of Chromatography

基　　金：湖北省自然科学基金资助项目(No.2006ABA165)

摘　　要：建立了鲫鱼肌肉中残留的辛硫磷的基质固相分散-高效液相色谱-二极管阵列检测(MSPD-HPLC-DAD)的分析方法。通过优化样品处理条件,确定选取0.50g鲫鱼肌肉样品与1.5g弗罗里硅土、0.5g无水硫酸钠混合研磨,并采用丙酮-正己烷溶液(体积比为40∶60)为洗脱剂,洗脱剂用量为25mL。优选的最佳色谱条件为:ODS色谱柱(250mm×4.6mm,5μm),流动相为甲醇-水(体积比为50∶50),流速0.6mL/min,检测波长270nm,进样量为20μL。在上述条件下,辛硫磷质量浓度在0.01～10mg/L范围内与响应信号呈良好的线性关系(r2=0.9994),检出限为3.3μg/kg;相对标准偏差为1.1%～6.3%(n=7);3个添加水平(0.05,0.1,1mg/kg)下得到的回收率为88%～112%。该方法操作简单,耗时少,精密度高,符合农残分析的要求。An analytical method was developed for the determination of phoxim residue in the muscle of crucian carp, which involved matrix solid-phase dispersion （MSPD） followed by high performance liquid chromatography （HPLC） with diode array detector. Under optimal conditions, 0.5 g tissue sample was dispersed with 1.5 g Florisil and 0.5 g anhydrous sodium sulphate, transferred to a cartridge. The cartridge was eluted with 25 mL acetone-hexane （40： 50, v/v）. The phoxim was separated on an ODS column （250 mm x4.6 mm, 5 μm） with methanol-water （50： 50, v/v） as the mobile phase at the flow rate of 0.5 mL/min, then detected by a diode array detector at 270 nm. The injection volume was 20 μL. The linear range of the method was 0.01 - 10 mg/L and the detection limit was 3.3 μg/kg. The average recoveries spiked at the levels of 0.05, 0. 1, 1 mg/kg ranged from 88% to 112% with the relative standard deviations （RSDs） of 1. 1% -6.3%. The method is quick, simple and can meet the requirement of the analysis of pesticide residues.

关 键 词：基质固相分散 高效液相色谱 辛硫磷 农药 残留 鲫鱼 

分 类 号：O658[理学—分析化学]