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本文建立了气相色谱-串联质谱联用仪(GC-MS/MS)同时测定大米中的41种农药残留的分析方法,即采用乙腈匀浆提取后,经基质固相萃取柱净化,乙腈定容,毛细管气相色谱柱程序升温分离,用GC-MS/MS(MRM)法确证分析,内标法定量。在0.02~1.5μg/ml质量浓度范围内,所有农药的线性相关系数均大于0.99,方法的定量限范围为0.0005~0.01mg/kg。分别在大米中进行3个添加水平(0.05、0.5、1.0μg/ml)的回收率实验,平均回收率为60.6%~125%,相对标准偏差为0.51%~3.92%,符合残留分析要求。该方法快速、灵敏、准确、高通量,具有良好的回收率和稳定性,运用串联质谱很好地消除了基质带来的干扰,可用于大米中农药残留的快速测定和确证。
In this paper, a method for simultaneous determination of 41 pesticide residues in rice by gas chromatography-tandem mass spectrometry (GC-MS / MS) has been developed. After acetonitrile was homogenized and purified by matrix solid phase extraction (SPE) , Capillary GC column temperature-programmed separation, GC-MS / MS (MRM) method to confirm the analysis, internal standard method. The linear correlation coefficients of all the pesticides were all greater than 0.99 in the range of 0.02 ~ 1.5μg / ml, and the limits of quantification of the method ranged from 0.0005 ~ 0.01mg / kg. The recoveries of three added levels (0.05, 0.5 and 1.0 μg / ml) in rice were respectively tested. The average recovery was 60.6% -125% and the relative standard deviation was 0.51% -3.92%, which met the requirements of residue analysis. The method is rapid, sensitive, accurate and high-throughput with good recovery and stability. The tandem mass spectrometry (MS) can eliminate the matrix interference and can be used for the rapid determination and confirmation of pesticide residues in rice.