文章摘要
张丹阳,贾昊,史小萌,王策,邓凯,耿岳,刘潇威,韦红.在线SFE-SFC-MS/MS在玉米粉农药多残留分析中的应用[J].农业环境科学学报,2021,40(10):2266-2276.
在线SFE-SFC-MS/MS在玉米粉农药多残留分析中的应用
Pesticide multiresidue analysis of corn flour using online SFE-SFC-MS/MS techniques
投稿时间:2021-05-06  
DOI:10.11654/jaes.2021-0530
中文关键词: 超临界流体萃取  超临界流体色谱  农药残留  玉米粉
英文关键词: supercritical fluid extraction  supercritical fluid chromatography  pesticide residue  corn flour
基金项目:国家自然科学基金项目(31801774)
作者单位E-mail
张丹阳 农业农村部环境保护科研监测所, 天津 300191  
贾昊 吉林农业大学资源与环境学院, 长春 130000  
史小萌 农业农村部环境保护科研监测所, 天津 300191  
王策 农业农村部环境保护科研监测所, 天津 300191  
邓凯 农业农村部环境保护科研监测所, 天津 300191  
耿岳 农业农村部环境保护科研监测所, 天津 300191 gengyue@caas.cn 
刘潇威 农业农村部环境保护科研监测所, 天津 300191 xwliu2006@163.com 
韦红 华标(天津)科技有限责任公司, 天津 300392  
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中文摘要:
      为评估玉米粉中农药多残留水平,采用在线超临界流体萃取-超临界流体色谱串联质谱法(SFE-SFC-MS/MS),建立了玉米粉中71种常用农药及其代谢物残留的精准定性定量分析方法。通过比较SFE提取及SFC分离分析参数,确定了最优的在线SFESFC-MS/MS条件,具体为:提取溶剂为超临界二氧化碳∶乙醇(91∶9,V/V),静态萃取和动态萃取时间均为5 min,动态萃取流速为5mL·min-1,分散剂无水硫酸镁和样品的比例为5∶1 (m/m),SFC改性剂为含0.1%甲酸的甲醇溶液,梯度洗脱,流速为1.5 mL·min-1,背压调节器A (Back pressure regulator A,BPRA)压力为14.8 MPa,柱温为40℃,柱后补偿溶剂为含0.1%甲酸的甲醇溶液,柱后补偿溶剂流速为0.05 mL·min-1。71种目标物在SFE-SFC-MS/MS上线性良好(R2>0.99),检出限和定量限分别为0.003~2.770 μg·kg-1和0.01~8.41 μg·kg-1。在1、10、100 μg·kg-1农药混标添加水平下,回收率为71.2%~124.6%、相对标准偏差为1.9%~30.5%。所建立的在线SFE-SFC-MS/MS法节省溶剂、操作简便省时、环境友好,可为玉米粉中农药多残留测定提供技术支撑。
英文摘要:
      In this study, to estimate the concentration of pesticide multiresidue in corn flour, an online supercritical fluid extraction method coupled with supercritical fluid chromatography tandem mass spectrometry(SFE-SFC-MS/MS) was established to facilitate the accurate qualitative and quantitative determination of 71 commonly used pesticide and metabolite residues in corn flour. By comparing different SFE extraction conditions and SFC chromatographic separation parameters, the following online SFE-SFC-MS/MS conditions were found to be optimal:the extraction solvent was a super critical CO2:ethanol mixture(91:9, V/V), static/dynamic extraction time was 5 min, dynamic extraction velocity was 5 mL·min-1, weight ratio of anhydrous magnesium sulfate(dispersant) and the sample was 5:1(m/m), SFC modifier was 0.1% formic acid methanol, gradient elution, flow rate was 1.5 mL·min-1, back pressure regulator A(BPRA) pressure was 14.8 MPa, column temperature was 40 oC, and the post-column compensation solvent was 0.1% formic acid methanol with a flow velocity of 0.05 mL·min-1. Good linearity was achieved(R2>0.99) for the 71 targets, with limits of detection and limits of quantification being 0.003~2.770 μg·kg-1 and 0.01~8.41 μg·kg-1, respectively. The recoveries were in the range of 71.2%~124.6% under fortification levels of 1, 10 μg·kg-1, and 100 μg·kg-1, with relative standard deviation ranging from 1.9%~30.5%. The online supercritical fluid extraction method was less solventconsuming, easier to operate, time saving, and environmentally friendly, which can be useful for detecting pesticide residues in corn flour.
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