固相萃取-高效液相色谱法测定蘑菇中咪鲜胺的残留量

Determination of Prochloraz Residues in Mushroom with Solid Phase Extraction-High Performance Liquid Chromatography

建立了蘑菇中咪鲜胺残留的固相萃取一高效液相色谱（SPE-HPLC）检测方法。对提取条件、固相萃取条件及仪器参数等进行了优化。提取液经C18和PSA固相萃取柱净化、浓缩后HPLC分离，紫外225nm检测。方法的检出限为0.038mg／kg，咪鲜胺在蘑菇样品中的添加回收率为82.6%-100.3%，变异系数是1.8％-9.2%，符合农药残留检测要求。

Determination of prochloraz residues in mushroom by solid phase extraction-high performance liquid chromatography （SPE-HPLC） has been conducted. In the method, acetonitrile and celite545 were added into representative sample, and the mixture was homogenized at ultra high speed. After filtration, the extract was purified by a liquid-liquid partitioning process with NaC1 solution and dichloromethane. The dichloromethane phase was evaporated to dryness, and the residue was dissolved with acetonitrile. Then, the organic phase was purified by PSA and C18 SPE tubes. At last, after filtrated with millipore filter, the prochloraz was determined by HPLC. The limit of detection was 0.038 mg/kg, the mean recoveries of prochloraz in the fortified mushroom samples ranged from 82.6% to 100.3%, and the relative standard deviations （RSDs） were in a range of 1.8%-9.2%. The proposed method is simple, rapid, economic and has good linearity.