水果蔬菜中7种新型生物农药残留检测方法研究

Study on the Determination of 7 New Biopesticides Residues in Fruits and Vegetables

建立一种全自动固相萃取-液质联用检测法测定水果蔬菜中7种新型生物农药残留。称取5.00 g样品,加入20 mL 2%乙酸,超声10 min,离心,上清液全部转移至25 mL比色管中,并用2%乙酸定容至25mL,取5 mL上清液上全自动固相萃取仪过MCX小柱净化,洗脱液蒸干并定容至1 mL,过0.20μm滤膜后上机测定。7种生物农药在4 min内全部出峰完毕,采用外标法定量,检出限均达0.010 mg/kg,在0.010~0.20mg/L范围内线性关系良好(r≥0.998),回收率80%~111.7%,RSD 1.1%~14.7%。该方法具有检出限低、前处理简单、检测速度快、定量准确等优点,能较好地满足实验室对水果蔬菜中生物农药残留检测的要求。

To establish an automatic solid phase extraction-liquid chromatography-mass spectrometry （LC-MS/MS） method for the determination of 7 new Biopesticides residues in fruits and vegetables# Weigh 5.00 g samples,add 20 mL 2 % HA,Ultrasonic for 10 min,Centrifuge,Transferred all Supernatant to 25 mL colorimetric tube, and with 2 % HA fixed volume to 25 mL, take 5 mL pass full-automatic solid phase extraction over MCX cartridge purification,the eluent evaporated to dryness and Seted the volume to 1 mL,passed 0.20 !m filter then tested, The 7 new Biopesticides showed all their peak within 4 min, the limit of detection was 0.010 mg/kg by external standard method,and the linearity was well in the range of 0.010-0.20 mg/L （ r !0.998）. The recovery rate was 8 0 % -111.7% and RSD was 1.1%-14.7%. This method has a low detection limit, simple pretreatment, fast detection and accurate quantification. It can meet the requirement of laboratory pesticide residues detection in fruits and vegetables Request.