高效液相色谱法测定食用菌中福美双残留量

Development of a HPLC-based Method for Determining Thiram in the Fruit Bodies of Edible Fungi

建立食用菌中福美双残留量的高效液相色谱(HPLC)检测方法。新鲜食用菌子实体样品粉碎后经二氯甲烷超声(53Hz)提取20min,离心(3320 g、5min),二氯甲烷经氮气吹干,甲醇定容后用HPLC测定。以等体积甲醇和0.1%甲酸水溶液为流动相,1mL/min等度洗脱,在0.05～10μg/mL范围内,福美双的峰面积与其浓度呈线性相关,R≥0.999,方法检出限为0.02mg/kg,添加回收率为79.4%～90.2%,变异系数为1.15%～7.51%%。

A method for determining thiram residues in fruit bodies of edible fungi based on high performance liquid chromatography（HPLC） is described.Fresh fruit bodies were cut mechanically into small pieces and extracted with dichloromethane for 20 min using ultrasound.After centrifugation（3320 g,5 min）,the supernatant was evaporated to dryness under nitrogen,the residue was re-dissolved in methanol,and samples were analyzed by HPLC.Separation was achieved at a flow rate of 1 mL/min using an isocratic elution with methanol and 0.1% aqueous formic acid solution（50/50,v/v）,and a good linear correlation（R≥0.999） between peak area and thiram concentration was obtained over the concentration range 0.05-10 μg/mL.The detection limit for thiram was 0.02 mg/kg,the recovery rate ranged between 79.4%-90.2%,and the variation coefficient varied between 1.15%-7.51%.