超高效液相色谱-串联质谱法测定小麦粉中福美双残留量

Determination of Thiram Residues in Wheat Flour by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立一种超高效液相色谱-串联质谱法(UPLC-MS/MS)测定小麦粉中福美双残留量的快速检测方法。小麦粉经甲醇超声提取,采用C18色谱柱分离,以乙腈+0.05%甲酸水体系进行梯度洗脱,质谱采用电喷雾正离子模式离子化,多反应监测模式,标准曲线外标法定量。福美双在5~100 ng/mL质量浓度范围内线性关系良好,相关系数大于0.999,定量限为0.02 mg/kg。小麦粉中福美双添加量为0.02、0.05、0.10 mg/kg时,福美双的平均加标回收率为70.52%~85.20%,相对标准偏差为8.74%~9.42%。该方法前处理过程简单,分析时间短,灵敏度和准确度高,适用于小麦粉中福美双残留量的批量快速检测。

A rapid analytical method for the determination of thiram residues in wheat flour was developed by UPLC-MS/MS.The sample was extracted by methanol,and then separated on a reversed phase C18 column using a gradient elution program of acetonitrile-0.05%formic acid aqueous solution.Qualitative analysis was performed with electrospray ionization in positive mode under multiple reaction monitoring mode.External standard curve method was used to quantify the residue concentrations.In the concentration range of 5-100 ng/mL for thiram,the calibration curves showed good linearity with correlation coefficients more than 0.999.The limit of quantitation of thiram in wheat flour was 0.02 mg/kg.At the spiked levels of 0.02,0.05,0.10 mg/kg,the average recoveries of thiram were 70.52%-85.20%,and the relative standard deviations of thiram were 8.74%-9.42%.The method is simple,rapid,and accurate,which can meet the batch rapid detection requirements of thiram residues in wheat flour.