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[目的]建立一种基质分散固相萃取测定小米籽粒、壳、植株和土壤中咪唑乙烟酸的残留方法。[方法]试样用pH=10缓冲液提取,甲酸调节pH值,二氯甲烷液液分配、石墨化炭黑(GCB)分散固相萃取净化,高效液相色谱-质谱测定。[结果]0.01~0.5 mg/kg添加水平范围内,咪唑乙烟酸在4种基质中平均添加回收率为76.6%~102.1%,相对标准偏差(RSD)为1.8%~14.5%,方法检出限(LOD)为0.003~0.005 mg/kg,定量限(LOQ)为0.01~0.05 mg/kg。[结论]该方法杂质干扰少,准确可靠,适用于对小米及土壤样品中咪唑乙烟酸残留检测。
[Objective] The research aimed to establish a matrix dispersive solid phase extraction method for the determination of imazethapyr residues in millet grains, shells, plants and soils. [Method] The samples were extracted with pH = 10 buffer solution, pH value was adjusted with formic acid, partitioned with liquid dichloromethane, dispersed solid phase extraction with graphite carbon black (GCB) and purified by high performance liquid chromatography - mass spectrometry. [Result] The average recoveries of imazethapyr within the range of 0.01-0.5 mg / kg were 76.6% -102.1% and the relative standard deviations (RSDs) were 1.8% ~ 14.5%. The detection limits (LOD ) Was 0.003 to 0.005 mg / kg, and the limit of quantification (LOQ) was 0.01 to 0.05 mg / kg. [Conclusion] This method has less impurity disturbance and is accurate and reliable, which is suitable for the determination of imazethapyr residues in millet and soil samples.