液相色谱–串联质谱法测定甘蓝中4-羟基百菌清的残留量

Determination of 4-Hydroxychlorothalonil Residues in Cabbage by Liquid Chromatography–Tandem Mass Spectrometry

建立液相色谱– 串联质谱法测定甘蓝中4- 羟基百菌清残留的方法.以乙腈提取样品中的4- 羟基百菌清,采用电喷雾负离子源（ESI–） 和多重反应监测（MRM） 模式测定,基质匹配标准工作曲线法定量.结果表明,甘蓝中4-羟基百菌清的质量浓度与其色谱峰面积呈良好的线性关系（r=0.999）,线性范围为1.0～100 μg/L,方法检出限为0.31μg/kg,定量限为1.0 μg/kg.在5,10,50 μg/kg 3个添加水平下,方法的回收率为88.0%～91.4%,测定结果的相对标准偏差为4.6%～7.2%（n=6）.该法简单、准确、快速、灵敏,符合法规残留限量监测要求.

The method for determination of 4-hydroxychlorothalonil residue in cabbage by liquid chromatography–tandem mass spectrometry was established. The sample was extracted with acetonitrile, electrospray negative ionsource（ESI–）, multiple reaction monitoring mode （MRM）, matrix–matched and standard curve method were applied tosamples analysis. The results showed that there was the good linear relationship（r=0.999） between chromatographic peakarea and mass concentration of 4-hydroxychlorothalonil residue in cabbage, the linear range was 1.0–100 μg/L, thedetection limit was 0.31 μg/kg,the quantification limit was 1.0 μg/kg. The method validation was carried out at 5,10,50μg/kg, the recoveries were from 88.0% to 91.4%, and the relative standard deviations of determination results were from4.6% to 7.2%（n=6）. The methods is simple, accurate, rapid, sensitive and suitable for monitoring the maximum residue limitof 4-hydroxychlorothalonil in cabbage.