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建立了小麦植株、麦粒、面粉、麦麸和土壤样品中氨氯吡啶酸的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品用丙酮提取,经N-丙基乙二胺(primary secondary amine,PSA)串联石墨化炭黑柱净化,以Agilent ZORBAX SB-C18色谱柱分离,以电喷雾电离串联质谱正离子多反应监测(multiple reaction monitoring,MRM)模式进行测定。结果表明:在0.01、0.1、0.5、1 mg/kg 4个添加水平下,氨氯吡啶酸在小麦植株、麦粒、面粉、麦麸和土壤中的平均回收率在78.9%~97.9%之间,相对标准偏差在3.6%~9.6%之间。该方法样品前处理简单、快速、分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于小麦和土壤中氨氯吡啶酸残留的检测。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed for the determination of climic acid in wheat, wheat, wheat flour and wheat bran. The samples were extracted with acetone and purified on a series of primary secondary amine (PSA) carbon black columns. The samples were separated on an Agilent ZORBAX SB-C18 column and detected by electrospray ionization tandem mass spectrometry positive ion multiple reaction monitoring ( multiple reaction monitoring (MRM) mode. The results showed that the average recoveries of clopidol in wheat plants, grains, flour, wheat bran and soil at the concentrations of 0.01, 0.1, 0.5 and 1 mg / kg were between 78.9% and 97.9% , The relative standard deviation of 3.6% ~ 9.6%. The method has the advantages of simple, rapid sample preparation, short analysis time, sensitivity, accuracy and precision meeting the requirements of pesticide residue detection, and is suitable for the determination of clopyralid residues in wheat and soil.