食品科学 ›› 2017, Vol. 38 ›› Issue (20): 273-278.doi: 10.7506/spkx1002-6630-201720040

• 安全检测 • 上一篇    下一篇

QuEChERS法前处理结合HPLC法测定苹果和土壤中二氰蒽醌的残留

秦旭,徐应明,赵立杰,黄青青,王林,孙约兵,梁学峰   

  1. (农业部环境保护科研监测所,天津 300191)
  • 出版日期:2017-10-25 发布日期:2017-09-29
  • 基金资助:
    天津市农业科技成果转化与推广项目(201502290)

Determination and Dissipation Kinetics of Dithianon Residue in Apple and Soil by Modified QuEChERS Coupled with HPLC

QIN Xu, XU Yingming, ZHAO Lijie, HUANG Qingqing, WANG Lin, SUN Yuebing, LIANG Xuefeng   

  1. (Agro-Environmental Protection Institute, Ministry of Agriculture, Tianjin 300191, China)
  • Online:2017-10-25 Published:2017-09-29

摘要: 建立苹果和土壤样品中二氰蒽醌的快速提取及高效液相色谱检测法。样品采用乙腈提取,改进的QuEChERS法净化,安捷伦Eclipse XDB-C18色谱柱进行分离,检测波长250?nm,基质匹配标准品外标法定量分析。二氰蒽醌在0.02~5.00?mg/L质量浓度范围内线性关系良好,在苹果和土壤中的平均回收率为74%~92%,相对标准偏差为1.02%~6.20%,最小检出量(RSN>3)为0.005?ng,检出限为0.02?mg/kg。田间实验结果表明,二氰蒽醌在苹果和土壤中的消解半衰期分别为3.8~12.6?d和1.0~8.3?d,在收获期苹果中的残留量均低于我国规定的最大残留限量5?mg/kg,推荐采收安全间隔期为14?d。

关键词: 二氰蒽醌, QuEChERS, 高效液相色谱, 苹果, 土壤, 残留

Abstract: A method was developed for the determination of dithianon residues in apple and soil by using high performance liquid chromatography (HPLC). The residues in samples were extracted with acetonitrile, cleaned up by a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method, separated on an Agilent Eclipse XDB-C18 column, and then analyzed by HPLC with variable-wavelength detection (VWD) at a wavelength of 250 nm. The analyte was quantified by the matrix-matched external standard method. Under the optimal conditions, the calibration curve showed good linearity in the range of 0.02–5.00 mg/L for dithianon. The average recoveries of dithianon were in the range of 74%–92%, with relative standard deviations (RSDs) of 1.02%–6.20%. The limit of detection (LOD, RSN > 3) of dithianon was 0.005 ng, and the limit of quantitation (LOQ) was 0.02 mg/kg. The half-life of dithianon was 3.8–12.6 and 1.0–8.3 days in apple and soil, respectively. At harvest, apple samples were found to contain dithianon levels below the maximum residue limit (MRL) in China (5 mg/kg). The harvest interval was recommended to be 14 days after the last application.

Key words: dithianon, QuEChERS, high performance liquid chromatography (HPLC), apple, soil, residue

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