摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法测定多种动物源性食品中地塞米松残留量的分析方法。方法样品经含1%甲酸的乙腈提取, QuEChERS方法净化后,以乙腈-0.1%甲酸水溶液为流动相,经PhenomenexKinetexF5色谱柱(100mm×3.0mm,2.6μm)分离,采用大气压化学电离源(atmosphericpressure chemicalionization,APCI),正、负模式同时扫描的离子化模式,多反应监测(MRM)模式采集,外标法定量。结果地塞米松在0.5~100 ng/mL浓度范围内线性良好,相关系数(r)为0.99946,检出限为0.10μg/kg;在3个加标水平下,平均回收率为73.2%~95.9%,精密度(n=6)为4.1%~10.7%。结论该方法简单、快速、稳定性高、重现性好,可满足多种动物源性食品中地塞米松残留量的检测。
Objective To establish a method for the determination of dexamethasone residues in various animal-derived foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile containing 1% formic acid, purified by QuEChERS method, and separated by Phenomenex Kinetex F5 column(100 mm×3.0 mm, 2.6 μm) with acetonitrile-0.1% formic acid aqueous solution as mobile phase. Using atmospheric pressure chemical ionization, the positive and negative modes were simultaneously scanned by ionization mode and multiple reaction monitoring(MRM) mode. The samples were collected and quantified by external standard method. Results The linearity of dexamethasone was good in the range of 0.5–100 ng/mL, the correlation coefficient(r) was 0.99946, and the detection limit was 0.10 g/kg. Under the 3 standard addition levels, the average recovery rate was 73.2%–95.9%, and the precision(n=6) was 4.1%–10.7%.Conclusion This method is simple, rapid, stable and reproducible, and can meet the requirements for the detection of dexamethasone residues in various animal-derived foods.
作者
曹丽丽
周鑫达
张爱芝
芦童
何海霞
王志强
忻璐琰
刘艳
CAO Li-Li;ZHOU Xin-Da;ZHANG Ai-Zhi;LU Tong;HE Hai-Xia;WANG Zhi-Qiang;XIN Lu-Yan;LIU Yan(Ningbo Institute for Food Control,Ningbo 315048,China)
出处
《食品安全质量检测学报》
CAS
2020年第15期5080-5087,共8页
Journal of Food Safety and Quality
关键词
QUECHERS
超高效液相色谱-串联质谱法
动物源性食品
地塞米松
大气压化学电离源
正负离子同扫
基质效应
QuEChERS
ultra performance liquid chromatography tandem mass spectrometry
animal derived food
dexamethasone
atmospheric pressure chemical ionization source
simultaneous scanning of positive and negative ions
matrix effect
