高效液相色谱-串联质谱法同时测定枸杞中31种农药残留
Determination of 31 pesticide residues in Chinese wolfcherry by high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定枸杞中31种农药残留的方法。枸杞经乙腈提取,Cleant TPH固相萃取柱净化,以C18色谱柱分离待测物,在电喷雾正离子化模式下,采用多反应监测(MRM)检测。结果表明,31种农药在1200μg/L的范围内线性关系良好,相关系数均大于0.995,方法检出限为0.657.1μg/kg,样品添加回收实验的平均回收率为69.7%112.1%,相对标准偏差为5.67%14.27%(n=6)。该方法简单准确,适用于枸杞中31种农药残留的同时检测。Abstract: A method for the simultaneous determination of 31 pesticide residues in Chinese wolfcherry by high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS) was developed. The samples were extracted with acetonitrile, cleaned up by Cleant TPH solid phase extraction column. The resulting samples were separated on a C18 column, and detected by multiple reactions monitoring ( MRM) under the condition of positive mode. The results showed that the linear calibration curves were obtained in the entire range ( 1200 μg/L) for all the above pesticides, with the correlation coefficients higher than 0.995, the detection limit was 0.65 ~ 7.1 μg/kg. For all the samples, the average spiked recoveries ranged 69.7%from 112.1%, and the relative standard deviations ( n = 6) were in the range of 5.67% ~ 14.27%.The method was easy and accurate, and can meet the requirement for the determination of the 31 pesticide residues in Chinese wolfcherry.