食品科学

• 分析检测 • 上一篇    下一篇

气相色谱法测定糙米和稻壳中丁虫腈残留量

史晓磊,井乐刚   

  1. 哈尔滨师范大学生命科学与技术学院,黑龙江 哈尔滨 150025
  • 出版日期:2013-12-25 发布日期:2014-01-03

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

SHI Xiao-lei,JING Le-gang   

  1. College of Life Science and Technology, Harbin Normal University, Harbin 150025, China
  • Online:2013-12-25 Published:2014-01-03

摘要:

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,R2=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。

关键词: 丁虫腈, 残留, 气相色谱, 糙米, 稻壳

Abstract:

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 + 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.

Key words: flufiprole, residue, gas chromatography (GC), brown rice, rice husk