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（MgSO4）、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0．01-2mg／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，啶虫眯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。
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 MgSO4,primary secondary amine（PSA） and C,8 with 1% 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, R^2 =0.9994,the LOQ of this method was 0.01mg/kg, which was below the MRL （0.5 mg/mL）. 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.
出处
《食品工业科技》
CAS
CSCD
北大核心
2015年第3期308-310,315,共4页
Science and Technology of Food Industry
基金
国家科技技术项目
科技基础性工作专项(2013FY110100)
关键词
啶虫脒
甘蓝
土壤
分散固相萃取
液相色谱串联质谱
acetamiprid
cabbage
soil
dispersive solid phase extraction （DSPE）
high performance liquidchromatography-mass spectrometry（HPLC-MS/MS）
