气相色谱法测定柑橘中螺螨酯残留量
目的 建立气相色谱-电子捕获检测器法(GC-ECD)测定柑橘中螺螨酯残留量的方法。方法 试样以乙腈为提取溶剂, 经涡旋提取高速离心后氮吹浓缩定容, 最后使用气相色谱电子捕获检测器测定。结果 螺螨酯在 0.01~2.0 mg/L浓度范围内呈现良好线性关系, R2 大于0.99, 在 0.1、0.5、1.0 mg/kg 三个添加浓度上回收率范围为91%~106.67%, 相对标准偏差小于5%, 方法检出限(LOD)(S/N=3)为0.05 mg/kg, 方法定量限(LOQ)(S/N=10)为0.10 mg/kg。结论 该方法前处理操作简单快速, 重复性好且灵敏度高, 满足国内外对柑橘中螺螨酯快速、准确检测的要求, 可应用于大量样品的定性定量分析。
Objective To establish a method for the determination of spirodiclofen residues in orange by gas chromatography with ECD detector(GC-ECD). Methods Samples were extracted with acetonitrile. After high speed centrifugation and concentrated by nitrogen flushing, samples were detected by GC-ECD. Results The method showed a good linearity in the range of 0.01~2.0 mg/L for spirodiclofen with R2 >0.99. The recoveries were in the range of 91%~106.67% at three spiked levels of 0.1, 0.5, and 1.0 mg/kg for spirodiclofen, and the relative standard deviations (RSDs) were less than5%. Value of detection limit (S/N=3) of the method was 0.05 mg/kg, and the limit of quantification (S/N=10) was 0.10 mg/kg. Conclusion The method is suitable for quantitative and qualitative analysis of spirodiclofen in a sufficient number of orange samples with sensitivity and repeatability, which can meet the fast and accurate detection requirements of spirodiclofen residues testing at home and abroad.
标题：气相色谱法测定柑橘中螺螨酯残留量
英文标题：Determination of spirodiclofen in oranges by gas chromatography
作者：
李东 衢州出入境检验检疫局
李卫兵 衢州出入境检验检疫局
祝子铜 衢州出入境检验检疫局
余琪 衢州出入境检验检疫局
徐佳文 衢州出入境检验检疫局
章应俊 衢州出入境检验检疫局
彭芳 衢州出入境检验检疫局
中文关键词:气相色谱法,螺螨酯,农药残留,柑橘,
英文关键词:gas chromatography,spirodiclofen,pesticide residue,orange,
发表日期：2014-06-21
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