摘要
本试验在QuEChERS方法前处理粮食样品(稻谷、小麦)的基础上,研究了不同改性剂、make up溶液、背压、make up泵流速和色谱柱温度对硫双威质谱响应的影响,建立了超临界流体色谱串联质谱的测定方法并进行方法学考察。结果表明:硫双威浓度在10~500μg/L范围内呈现良好的线性关系(相关系数R^(2)>0.991),定量限为15μg/kg,分别选取稻谷、小麦进行测定,在添加3个浓度水平下测得加标回收率在71.2%~103.5%,相对标准偏差为2.64%~10.68%(n=6)。采用SFC-MS/MS方法检测硫双威较LC-MS/MS检测更具有环保性(低溶剂)、成本低的优势。
Based on the pretreatment of grain samples(rice and wheat) with QuEChERS method,this experiment studied the effects of different modifiers,make up solution,back pressure,make up pump flow rate and column temperature on the mass spectrum response of thiodicarb.A new method for the determination of thiodicarb in grain by supercritical fluid chromatography-tandem mass spectrometry was established and the methodology was investigated.The results showed that the calibration curves for thiodicarb demonstrated good linearity in the range of 10~500 μg/L,with the correlation coefficients better than 0.991,and the quantification limits was 15 μg/kg.The average recoveries of thiodicarb at the spiked levels of 50,100,200 μg/kg ranged from 71.2%~103.5% with RSDs of 2.64%~10.68%(n=6).Conclusion Compared with LC-MS/MS,the SFC-MS/MS method has the advantages of environmental protection(lower solvent) and lower cost.
作者
谢婷婷
Xie Tingting(Institute of Grain and Oil Quality Supervision and Test of Fujian Province,Fuzhou 350012)
出处
《粮食与食品工业》
2023年第4期48-54,共7页
Cereal & Food Industry
关键词
硫双威
超临界流体色谱串联质谱联用技术
超高效液相色谱串联质谱联用技术
thiodicarb
supercritical fluid chromatography mass spectrometry
high perform ance liquid chromatography tandem triple quadrupole mass spectrometry
作者简介
谢婷婷,女,1988年出生,工程师,研究方向为农产品加工及贮藏工程。
