中国农业机械化科学研究院集团有限公司 主管

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多离子反应监测结合UPLC-MS/MS法测定柑橘中22种防腐保鲜剂残留

Determination of 22 preservative residues in citrus by UPLC-MS/MS with multiple ion reaction monitoring

  • 摘要: 建立超高效液相色谱质谱联用法测定柑橘中22种防腐保鲜剂残留的方法。样品经QuEChERS法处理,通过UPLC BEH C18色谱柱分离,用0.01%甲酸水−0.01%甲酸甲醇洗脱,在电喷雾正离子源多反应监测模式(MRM)下测定,通过外标法定量。结果表明,5~200 μg/L质量浓度22种防腐保鲜剂线性良好(相关系数>0.997),方法检出限0.10~0.60 μg/kg,10、20、100 μg/kg添加水平的加标回收率86.3%~116.6%,相对标准偏差(n=6)0.6%~4.8%。利用多离子反应监测目标化合物的离子丰度比,确证所有检出样品均为阳性。该方法具有操作简便、灵敏度高、重现性好的优点,适用于柑橘中22种防腐保鲜剂残留同时测定。

     

    Abstract: A method for determining residues of 22 preservative in citrus by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Samples were extrated by QuEChERS method, separated on an UPLC BEH C18 column, eluted with mobile phase of 0.01% formic acid in water and 0.01% formic acid in methanol.Target compounds were detected under multiple reaction monitoring(MRM)mode with an electrospray ionization positive ion source.Quantification was performed using an external standard method.Results showed that 22 preservatives exhibited good linearity(correlation coefficient >0.997)across concentrations ranging within 5~200 μg/L, method detection limits ranged within 0.10~0.60 μg/kg.Spiked recovery rates at addition levels of 10, 20, and 100 μ g/kg ranged within 86.3%~116.6%, with relative standard deviations(n=6)within 0.6% ~4.8%.By using multiple ion reactions to monitor ion abundance ratio of target compounds, all detected samples were confirmed as positive.This method has advantages of simple operation, highly sensitive, and good reproducibility, making it suitable for simultaneous determination of 22 preservative residues in citrus.

     

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