粮谷中三环唑残留量的检测方法研究

Determination of Tricyclazole Residues in Cereals by LC-MS / MS Method

建立了玉米、大麦、糙米、大米、小麦5种粮谷基质中三环唑残留量的液相色谱-质谱／质谱检测方法。样品经丙酮涡旋振荡提取，再经中性氧化铝固相萃取柱净化后，由液相色谱-质谱／质谱检测，外标法定量。方法的定量限为0．01mg／kg，标准品浓度在2．5～80ng／mL呈良好的线性关系，相关系数大于0．99。粮谷样品在0．01、0．02和3．00mg／kg添加水平的回收率范围分别为72．1％～95．6％、73．0％～95．4％、80．1％～99．2％，相对标准偏差范围在2．2％-7．4％。本方法方便、快速、溶剂消耗低、灵敏度高、回收率稳定，可以满足进出口粮谷中三环唑残留量的检测需求。

A high performance liquid chromatography coupled tandem mass spectrometry （HPLC -MS/MS） method was established to detect tricyclazole residue in corn, barley, brown rice, rice and oat. The sample was extracted by acetone and be cleaned up by N - A12 03 solid phase extraction column. The extract had been determined by HPLC - MS/MS and quantified by external standard method. The quantization limit was 0. 010 mg/kg. The calibration curve showed favorable linearity in range of 2.5 - 80 ng/mL with relative coefficient above 0.99. The average recoveriesof tricyclazole in cereals at three spiked concentration levels of 0.01,0.02 and 3.00 mg/kg were 80. 1% 99.2% ,respectively ,with relative standard deviations of 2.2- 7.4%. The method is easy ,fast,low solvent consumption, with high sensitivity, stable recovery, which can meet the requirements for determination of tricyclazole in impor- ted and exported cereals.