摘要
建立了超高效液相色谱串联质谱(UPLC-MS/MS)法测定番茄和土壤中咯菌腈残留的检测方法。用乙腈水溶液提取样品中的咯菌腈,经PSA(N-丙基乙二胺)和硅镁型吸附剂净化后,以C18柱为分析柱、乙腈-甲酸水溶液为流动相,采用超高效液相色谱串联质谱多反应监测,电喷雾负离子源,外标法定量。咯菌腈在0.01～2.00 mg·L-1范围内与峰面积呈良好的线性关系,线性方程为y=3 412.6x+163.95,r2=0.999 5。向对照番茄果实和对照土壤中分别添加咯菌腈标样,添加水平分别为0.01、0.10、2.00 mg·kg-1时,平均回收率分别为95.96%～103.17%和88.21%～106.88%,相对标准偏差分别为1.8%～4.6%和1.1%～6.2%。番茄和土壤中咯菌腈的检出限均为0.4μg·kg-1,定量限分别为1.4μg·kg-1和1.3μg·kg-1。该方法简单、快速,准确度和灵敏度都较高,适用于番茄和土壤中咯菌腈的残留分析。
An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of fludioxonil residues in tomato and soil samples. The samples were extracted with aqueous acetonitrile, and then purified by primary secondary amine(PSA)and Florisil. Chromatographic separation was performed on an ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7 μm)with a mobile phase composed of aqueous solution(containing 0.1% formic acid)and acetonitrile in gradient elution. Mass spectrometric detection was conducted in negative electrospray ionization (ESI) with multiple reaction monitoring(MRM)mode. The quantification of fludioxonil was performed using the external standard method. An excellent linear relationship between peak area(y)and mass concentration (x) of fludioxonil was obtained in the range of 0.01~2.00 mg·L^-1. The linear equation was y=3 412.6x+163.95, and the correlation coefficient(r^2)was 0.999 5. At three fortification levels of 0.01, 0.10 mg·kg^-1and 2.00 mg·kg^-1, the average recovery rates of fludioxonil in the tomato and soil samples were in the ranges of 95.96%~103.17% and 88.21%~106.88%, with the relative standard deviations(RSD)of 1.8%~4.6% and 1.1%~6.2%, respectively. The limit of detection(LOD)for both the tomato and soil samples was 0.4 μg·kg^-1.The limits of quantification (LOQ) for them were 1.4 μg·kg^-1and 1.3 μg·kg^-1, respectively. This method is simple, rapid, accurate and sensitive, and is suitable for the analysis of fludioxonil residues in tomato and soil.
作者
张一汀
井乐刚
张晓波
董见南
刘峰
陈国峰
ZHANG Yi-ting;JING Le-gang;ZHANG Xiao-bo;DONG Jian-nan;LIU Feng;CHEN Guo-feng(College of Life Science and Technology,Harbin Normal University,Harbin 150025,China;Safety and Quality Institute of Agricultural Products,Heilongjiang Academy of Agricultural Sciences,Harbin 150086,China)
出处
《农业环境科学学报》
CAS
CSCD
北大核心
2019年第1期243-248,共6页
Journal of Agro-Environment Science
基金
黑龙江省自然科学基金项目(C201236)
哈尔滨市科技创新人才研究专项(RC2017QN020016)~~
关键词
咯菌腈
番茄
土壤
残留
超高效液相色谱串联质谱
fludioxonil
tomato
soil
residue
ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
