超高效液相色谱-串联质谱法测定八角中甲霜灵和抗蚜威的残留量

Determination of metalaxyl and pirimicarb residues in star anise by ultra performance liquid chromatographys-tandem mass spectrometry

中文关键词:  甲霜灵  抗蚜威  超高效液相色谱-串联质谱法  八角

英文关键词:metalaxyl  pirimicarb  ultra high performance liquid chromatography-tandem mass spectrometry  star anise

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测八角中甲霜灵和抗蚜威残留量的分析方法。方法 利用乙腈/水混合溶剂提取, 盐析后取上清液, 通过QuEChERS方法净化, 用超高效液相色谱-串联质谱测定, 外标-标准曲线法定量。结果 甲霜灵和抗蚜威在0.001~0.05 mg/L范围内具有良好的线性关系, 相对系数均大于0.999。3个质量水平的添加0.01、1、5 mg/kg, 甲霜灵回收率为83.4%~105%, 相对偏差为1.2%~6.5%。抗蚜威回收率为81.3%~105%, 相对偏差为1.3%~2.7%。结论 该方法简便、快捷、分离净化效果好, 灵敏度高, 精密度和准确度均达到农药残留检测要求。

英文摘要:

      Objective To establish a method for the determination of metalaxyl and pirmicarb residues in star anise by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The mixture was extracted with acetonitrile/water mixed solvent, and the supernatant was extracted after salting out, purified by QuEChERS method, determined by ultra high performance liquid chromatography-tandem mass spectrometry, and quantified by external standard-standard curve method. Results There was a good linear relationship between methanolin and aphid in the range of 0.0010.05 mg/L, and the relative coefficient was greater than 0.999. The recovery rate of metoxiflin was 83.4%105% with the three addition at quality levels of 0.01, 1 and 5 mg/kg, and the relative deviation was 1.2%6.5%. The recovery rate of aphid resistance was 81.3%105%, and the relative deviation was 1.3%2.7%. Conclusion The method is simple, rapid with good separation and purification effect, high sensitive, the precise and accuracy meet the requirements of pesticide residues detection.