气相色谱法测定糙米和稻壳中丁虫腈残留量

Determination of Flufiprole Residues in Brown Rice and Rice Husk by GC

建立气相色谱法测定糙米和稻壳中丁虫腈残留的方法。样品中丁虫腈经乙腈溶液提取、弗罗里硅土柱净化、DB-1MS毛细管气相色谱柱分离，采用电子捕获检测器检测。丁虫腈在0．01-0．2mg／L范围内与峰面积呈良好线性关系，线性方程为：y=1×106x＋3677．6，R^2=0．9958。向空白糙米、空白稻壳中分别添加丁虫腈标样，使其添加量分别为0．01、0．02、0．10mg／kg时，平均回收率分别在84．2％～104．1％、89．7％-97.3％之间，相对标准偏差分别在5．2％～12．7％、4.3％～15．5％之间。糙米和稻壳中丁虫腈残留的最低检测限均为0．01mg／kg。该方法简便、快速、灵敏，适合于糙米和稻壳中丁虫腈的残留分析。

A method for determining flufiprole residues in brown rice and rice husk was proposed by gas chromatography （GC）. The flufiprole residues in samples were extracted with aqueous acetonitrile, cleaned up on a Florisil column, separated using gas chromatography equipped with a DB-1MS capillary column and detected with an electron capture detector. An excellent linear relationship between flufiprole concentration （x） in the range of 0.01-0.2 mg/L and peak area （y） was achieved. The linear equation was y = 1 × 106x q- 3677.6, with a coefficient of determination of was 0.9958. For brown rice, the mean recoveries of the method varied from 84.2% to 104.1% with a relative standard deviation ranging from 5.2% to 12.7% at three spiked levels of 0.01, 0.02 mg/kg and 0.1 mg/kg. For rice husk, the mean recoveries varied from 89.7% to 97.3% with a relative standard deviation ranging from 4.3% to 15.5% at three spiked levels of 0.01, 0.02 mg/kg and 0.1 mg/kg. The limit of detection for both brown rice and rice husk was 0.01 mg/kg. This method is simple, rapid, sensitive, and can be used for the determination of flufiprole residues in brown rice and rice husk.