超高效液相色谱-四极杆-飞行时间质谱法快速筛查农药制剂中非法添加的化学杀菌剂

建立了超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOF MS)快速筛查农药制剂中35种非法添加化学杀菌剂的方法.农药制剂样品经甲醇超声溶解提取后,采用Zorbax C18色谱柱(100 mm×1.8 mm,2.1μm)进行分离,以0.1%甲酸-乙睛作为流动相进行梯度洗脱,采用正离子全扫描模式进行分析.在所建立的条件下,35种杀菌剂在0.2,0.4和2.0 mg/kg水平下的添加回收率为81.0%~101.3%,相对标准偏差为1.0%~4.4%.在100份样品有6份样品中筛查出添加了化学杀菌剂,并进行了含量分析.本方法分析效率高,结果准确可靠,适用于农药制剂中非法添加化学杀菌剂的定性筛查.

Rapid Screening of Illegally Added Chemical Fungicide in Pesticide Formulations by Ultra Performance Liquid Chromatography- Quadrupole-Time of Flight Mass Spectrometry

A method of ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry ( UPLC-Q-TOF MS) was developed to determine 35 kinds of illegally added chemical fungicides in pesticide formulations. The samples were pretreated based on the ultrasonic extraction by the solvent of methanol, and then separated on a Zorbax C18(100 mm×1. 8 mm, 2. 1 μm) column by a gradient elution with 0. 1% formic acid aqueous solution and acetonitrile as the mobile phase. The mass spectrometer was operated under positive mode. Under the optimal conditions, the recoveries at three spiked levels (0. 2, 0. 4, and 2. 0 mg/kg) were in the range of 81. 0%-101. 3% and the RSDs were 1. 0%-4. 4%. Based on the developed method, 100 samples were analyzed, and among which 6 samples were screened out chemical fungicides. The proposed method was high-efficient, accurate and reliable for the qualitatively screening of illegaly added chemical fungicides.