摘要
建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速测定食品中双胍三辛烷基苯磺酸盐、双炔酰菌胺、噁霉灵3种杀菌剂的方法,样品采用乙腈(含0.1%乙酸)提取,Hypersil GOLD C18(100 mm×2.1 nm,1.8μm)分离,用甲醇和10 mmol/L乙酸铵(含0.1%甲酸)水溶液作为流动相进行梯度洗脱,正离子模式扫描。化合物一级质谱的分辨率为70000。通过高分辨质谱Full-MSdd MS^2正离子扫描模式进行定性和定量分析。实验结果表明,3种目标化合物在(5～500)mg/L范围内具有良好的线性,线性相关系数均大于0.999,检出限(LOD)分别为8、1.5、1.5μg/kg,定量限(LOQ)分别为25、5、5μg/kg。平均回收率为75%～106%,相对标准偏差为2.1%～5.9%,该方法具有准确、简便、快速的特点,可用于食品中3种杀菌剂的快速定性筛查和定量分析。
A method for rapid screening and quantification of 3 fungicides residues(Iminoctadine trialbesilate. Mandipropamid and Hymexazol) in foods by ultra performance liquid chromatography(UPLC)-quadrupole/electrostatic field orbitrap high resolution mass spectrometry was established. The samples were extracted with acetonitrile, and separated on an Hypersil GOLD C18 column(100 mm×2.1 nm, 1.8 μm) with methano(1~10)mmol/L ammonium acetate solution as mobile phases by gradient elution. The positive mode was used in the MS detection. The resolution of the precursor mass was 70000. The results indicated that the linearity of 3 fungicides ranged from 5 mg/L to 500 mg/L with the correlation coefficients greater than 0.999. The limits of detection were confirmed by spiked samples, and were 8, 1.5 and 1.5 μg/kg for the 3 fungicides. The recoveries were in the range of 75% to 106%, with the relative standard deviations in the range of 2.1%~5.9%. This method is accurate, simple and rapid, and can be used in rapid screening and quantitative analysis of the 3 fungicides residues in foods.
作者
李云飞
杨玲春
殷红
朱红玉
王英
张薇
张银
陈宏仙
LI Yunfei;YANG Lingchun;YIN Hong;ZHU Hongyu;WANG Ying;ZHANG Wei;ZHANG Yin;CHEN Hongxian(Technical Center of Yunnan Entry-Exit Inspection and Quarantine Bureau,Kunming 650051)
出处
《食品科技》
CAS
北大核心
2018年第12期336-340,共5页
Food Science and Technology
基金
"十三五"国家重点研发计划项目(2017YFF0211000)
关键词
超高效液相色谱
静电场轨道阱高分辨质谱
杀菌剂
食品
ultra performance liquid chromatography (UPLC)
quadrupole/electrostatic field orbitrap high resolution mass spectrometry
fungicides
food
