蜂蜜中氟胺氰菊酯残留量的测定

DETERMINATION OF FLUVALINATE RESIDUE IN HONEY BY GAS CHROMATOGRAPHY

蜂蜜样品经过碱解、溶剂提取、固相萃取净化处理后 ,用配有双柱双电子捕获检测器的气相色谱仪测定其中氟胺氰菊酯的残留量。利用气相色谱 -质谱联用仪验证了氟胺氰菊酯的两个旋光异构体的存在。通过 0 .0 1、0 .1和 0 .2mg/kg 3个水平的添加实验 ,在HP - 5 0 + 和HP - 1色谱柱上测定 ,回收率分别为 86 .3% 95 .37%、82 .83% 91.4 % ,检出限分别为 0 .0 0 7、0 .0 0 3mg/kg ,RSD <5 % (n =3)。

Fluvalinate residue in honey was determined by gas chromatography (GC) with twin columns and twin electron capture detectors (ECD) after honey sample was prepared by alkalizing with 1 mol/L NaOH solution, extracting with acetone-hexane (1∶2), and cleaning up with a Florisil solid-phase extraction (SPE) cartridge. Two optical isomers of fluvalinate were separated completely with HP-50^(+) and HP-5MS columns and confirmed by gas chromatography-mass spectrometry. Recovery experiments were carried out at three levels 0.01, 0.1 and 0.2 mg/kg. Average recoveries were in the range of 86.3% ~ 95.37% and 82.83% ~ (91.4)% respectively for the HP-50^(+) and HP-1 column. The limits of detection were 0.007 mg/kg and 0.003 mg/kg respectively. The relative standard deviation coefficient of variation (RSD) was less than 5% (n=3).