摘要
建立一种采用固相萃取净化提取蓝莓等浆果中的氟啶虫酰胺和溴氰虫酰胺,液相色谱-质谱法定性定量检测的分析方法。蓝莓等浆果均质后,采用乙腈提取,固相萃取净化、富集,收集液经氮吹近干,甲醇定容,液相色谱-质谱仪定性定量检测。结果表明:氟啶虫酰胺和溴氰虫酰胺在0.02~1.0μg/m L质量浓度范围内线性关系良好,相关系数(R2)均大于0.995;氟啶虫酰胺和溴氰虫酰胺检出限分别为0.0013 mg/kg和0.0021 mg/kg;加标回收率(0.02,0.1和0.5μg·m L^-1)分别在87.7%~90.7%和88.6%~103.4%之间;重复性与精密度相对标准偏差均在5.0%以内(n=6)。该方法具有灵敏度高、前处理简单、重复性好等优点,适用于蓝莓等浆果中氟啶虫酰胺和溴氰虫酰胺的检测。
A HPLC/MS method for the extraction and purification of flonicamid and cyanuramide from blueberry and other berries by solid phase extraction(SPE)was developed.After homogenized,blueberry samples were extracted by acetonitrile,then purified and extracted by SPE.The extracted solution was blown nearly dry by nitrogen,then fixed to 1 m L by methanol.Samples were detected qualitatively and quantitatively by HPLC/MS.The results showed that flonicamid and cyanuramide pesticides residues showed good linear relationships in the range 0.02-1.0μg/m L,and correlation coefficients(R2)were all above 0.995.Detection limits were as follows:flonicamid 0.0013 mg/kg and cyanuramide 0.0021 mg/kg.The recoveries of flonicamid and cyanuramide(0.02,0.1 and 0.5μg·m L^-1)were ranged from 87.7%-90.7%and 88.6%^-103.4%,respectively.The RSDs of reproducibility and precision were all below 5.0%(n=6).This method had the advantages of high sensitivity,simple pretreatment and good repeatability,and it was suitable for the detection of flonicamid and cyanamide in blueberries and other berries.
作者
毕思远
曹涛
朱志强
林燕翠
甘慧
BI Siyuan;CAO Tao;ZHU Zhiqiang;LIN Yancui;GAN Hui(Hebei Medical University,Public Health Colleg,Shijiazhuang 050017;Hebei Key Laboratory of Environment and Human Health,Shijiazhuang 050017;Guangdong Quick Test Technologies Co.,Ltd.,Dongguan 523843;Shenzhen Huizhi Technologies Co.,Ltd.,Shenzhen 518101)
出处
《食品工业》
CAS
北大核心
2020年第9期289-292,共4页
The Food Industry
基金
国家博士后基金面上项目二等资助(No.2017M611382)。
