高效液相色谱-串联质谱法测定小麦和土壤中氨氯吡啶酸的残留量

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。

Determination of picloram residues in wheat and soil by high performance liquid chromatography-tandem mass spectrometry

A method was developed for residue determination of picloram in wheat plants,grain,flour,wheat bran and soil by using high performance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS).The residues of picloram in wheat and soil samples were extracted by acetone and cleaned up by primary secondary amine(PSA) connected with graphite carbon column,and then analyzed by HPLC-MS/MS in multiple reaction monitoring(MRM) mode via positive electrospray ionization with an Agilent ZORBAX SB-C₁₈ as the analytical column.Results showed that at fortified levels of 0.01 to 1 mg/kg,the average recoveries of picloram in wheat plants,grain,flour,wheat bran and soil were from 78.9% to 97.9%,and RSD were from 3.6% to 9.6%.The method is simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.The method is applicable to confirm the residues of picloram in wheat and soil.