QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留

Determination of 4 pesticide residues in bamboo shoots by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

目的建立检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法。方法前处理采用QuEChERS方法,乙腈为提取液,N-丙基乙二胺(PSA)为净化剂,结合液相色谱-质谱联用技术,正离子多反应监测(MRM)模式进行检测,外标法定量。结果吡虫啉、茚虫威、辛硫磷和克百威4种农药在0.5～20.0 ng/ml范围呈良好的线性关系,相关系数(r^2)均大于0.991,在4～40μg/kg加标范围内,4种农药的回收率为72.4%～92.8%,精密度为1.5%～9.2%,方法的检出限为0.4μg/kg,定量限为1.2μg/kg。结论建立了适用于检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法,该方法准确、灵敏、高效、简便。

Objective A simple and rapid QuEChERS-high performance chromatography-tandem mass spectrometric method was developed for the determination of 4 pesticides, imidacloprid, indoxacarb, phoxim and carbofuran, in bamboo shoots. Methods The residues were extracted from the bamboo shoots with acetonitrile and cleaned up with N-propyl ethylenediamine（PSA）, then detected by liquid chromatography-tandem mass spectrometry under multiple reaction monitroring mode（MRM）, and quantified by matrix-match calibration curves. Results The recoveries in samples were between 72.4%-92.8% at three spiked levels from 4 to 40 μg/kg, with relative standard deviations of 1.5%-9.2%（n=3）. The limits of detection（LOD） of four pesticides were 0.4 μg/kg, while limits of quantification（LOQ） were 1.2 μg/kg. The linear ranges were 0.5-20.0 ng/ml and the correlation coefficients（r^2） were above 0.991. Conclusion The method of QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry was accurate, sensitive, simple and convenient for the determination of the 4 pesticide residues, imidacloprid, indoxacarb, phoxim and carbofuran, in bamboo shoots.