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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,R~2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 gas chromatography-electron capture detector (GC-ECD) method for the determination of citrulline residues in citrus. Methods Acetonitrile was used as the extraction solvent. After vortex extraction and high-speed centrifugation, the nitrogen was concentrated and concentrated. Finally, the sample was determined by gas chromatography electron capture detector. Results Spirodiclofen had good linearity in the concentration range of 0.01-2.0 mg / L, R ~ 2 was greater than 0.99, and the recoveries ranged from 91% to 106.67% at three concentrations of 0.1, 0.5 and 1.0 mg / kg, The standard deviation was less than 5%, and the limit of detection (LOD) was 0.05 mg / kg. The limit of quantification (LOQ) was 0.10 mg / kg. Conclusion The pretreatment method is simple, rapid, reproducible and sensitive. It can meet the rapid and accurate detection of spirodiclofil in citrus at home and abroad, and can be applied to qualitative and quantitative analysis of a large number of samples.