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中国精品科技期刊2020
秦迪, 杨鑫, 王静, 金芬, 邵华, 魏闪闪. 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[J]. 食品工业科技, 2015, (03): 308-310. DOI: 10.13386/j.issn1002-0306.2015.03.056
引用本文: 秦迪, 杨鑫, 王静, 金芬, 邵华, 魏闪闪. 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[J]. 食品工业科技, 2015, (03): 308-310. DOI: 10.13386/j.issn1002-0306.2015.03.056
QIN Di, YANG Xin, WANG Jing, JIN Fen, SHAO Hua, WEI Shan-shan. Determination of acetamiprid in soil and cabbage by dispersive solid phase extraction and high performance liquid chromatography tandem mass spectrometry[J]. Science and Technology of Food Industry, 2015, (03): 308-310. DOI: 10.13386/j.issn1002-0306.2015.03.056
Citation: QIN Di, YANG Xin, WANG Jing, JIN Fen, SHAO Hua, WEI Shan-shan. Determination of acetamiprid in soil and cabbage by dispersive solid phase extraction and high performance liquid chromatography tandem mass spectrometry[J]. Science and Technology of Food Industry, 2015, (03): 308-310. DOI: 10.13386/j.issn1002-0306.2015.03.056

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

  • 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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