分散固相萃取-高效液相色谱串联质谱测定甘蓝及土壤中的啶虫脒
Determination of acetamiprid in soil and cabbage by dispersive solid phase extraction and high performance liquid chromatography tandem mass spectrometry
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摘要: 建立了甘蓝和土壤中啶虫脒的分散固相萃取-高效液相色谱串联质谱检测方法,该方法以1%乙酸乙腈为提取溶剂（1∶99,v/v）,以无水硫酸镁（Mg SO4）、十八烷基键合硅胶（C18）和N-丙基乙二胺（PSA）富集净化,0.1%甲酸-水和甲醇梯度洗脱,C18柱分离,HPLC-MS/MS测定。方法线性范围0.012mg/L,相关系数为0.9994,定量限（LOQ）为0.01mg/kg。在0.05、0.5、1.0mg/kg加标浓度下,啶虫脒在甘蓝中的回收率为84.8%107%,在土壤中的回收率为96.5%115%,相对标准偏差小于10.92%。该方法能够满足甘蓝及土壤中啶虫脒残留限量检测要求。Abstract: A method using dispersive solid phase extraction( DSPE) cleanup followed by high performance liquid chromatography- mass spectrometry( HPLC- MS) has been established for determination of acetamiprid in soil and cabbage.In this method,the clean- up was carried out using Mg SO4,primary secondary amine( PSA) and C18with1% acetic acid- acetonitrile as extract solvent.0.1% formic acid in water and methanol were used as mobile phase,C18 chromatographic column was used to separation in determinating samples on HPLC- MS.In the range of 0.01~2mg / L,the good linear relationship was showed between concentration and peak area,R2= 0.9994,the LOQ of this method was 0.01 mg / kg,which was below the MRL( 0.5mg / m L). At the spiked levels of 0.05,0.5,1.0mg / kg,the recoveries of acetamiprid were 84.8% ~ 107% in cabbage and 96.5% ~ 115% in soil,and the relative standard deviation( RSD) was less than 10.92%. This method can meet the requirements of the limited determination of acetamiprid residues in cabbage and soil.
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