豆粉中31种杀菌剂残留的UPLC-MS/MS测定法
Determination of 31 fungicides residues in soybean powder by UPLC-MS/MS
张波 1郭二菱 2黄笑晨 2郭爱静 2王可2
作者信息
- 1. 承德市食品药品检验检测中心食品检验室,河北承德 067000
- 2. 石家庄市疾病预防控制中心,石家庄市化学毒物检测及风险预警技术创新中心,河北石家庄 050011
- 折叠
摘要
目的 建立 QuEChERS(quick、easy、cheap、effective、rugged、safe)结合超高效液相色谱-串联质谱(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)测定豆粉中31种苯并咪唑类和三唑类杀菌剂残留的方法.方法 乙腈提取豆粉样品,用十八烷基键合硅胶(C18)填料和无水硫酸镁净化上清液后氮吹干.待测样品经Kinetex@F5100A(3.0×100 mm,2.6 µm)柱子进行分离,以0.1％甲酸水溶液(A相)和甲醇(B相)作为流动相,电喷雾正离子源(electrospray ionization,ESI+)模式电离,多反应监测(multiple reaction monitoring,MRM)模式进行检测,基质匹配法定量分析.结果 31种杀菌剂浓度为0.1～100 μg/L,呈良好的线性关系(r＞0.999),各杀菌剂检出限为0.01～1.03 µg/kg,定量限为0.01～3.44 μg/kg,在3个不同浓度下的加标平均回收率为71.3％～118.7％,相对标准偏差为0.4％～9.9％.结论 该方法操作简便,适用于大豆样品中31种苯并咪唑类和三唑类杀菌剂的高通量快速检测.
Abstract
Objective To establish a QuEChERS(quick,easy,cheap,effective,rugged,safe)method combined with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)for detecting residues of 31 benzimidazole and triazole fungicides in soybean powder.Methods The soybean powder samples were extracted using acetonitrile,the supernatant was purified using octadecyl bonded silica gel(C18)and anhydrous magnesium sulfate,and then blow dry with nitrogen.The samples were separated using Kinetex@F5 100A(3.0×100 mm,2.6 μm)with mobile phases consisting of 0.1％formic acid aqueous solution(phase A)and methanol(phase B).The electrospray ionization(ESI+)mode was used for ionization,while detection was conducted using multiple reaction monitoring(MRM).The quantitative detection was performed utilizing the matrix matching method.Results Totally 31 fungicides exhibit a good linear relationship(r＞0.999)within the mass concentration range of 0.1-100 μg/L.The limits of detection of the fungicides were 0.01-1.03 μg/kg,the limits of quantitation were 0.01-3.44 μg/kg.The average recovery rate of spiked samples at three different concentrations was 71.3％-118.7％,and the relative standard deviations were 0.4％-9.9％.Conclusion The method is uncomplicated and suitable for rapidly detecting 31 triazole and benzimidazole fungicides in soybean powder samples.
关键词
超高效液相色谱-串联质谱/苯并咪唑类杀菌剂/三唑类杀菌剂/豆粉/QuEChERSKey words
Ultra performance liquid chromatography tandem mass spectrometry/Benzimidazole fungicides/Triazole fungicides/Soybean powder/QuEChERS引用本文复制引用
基金项目
河北省医学适用技术跟踪项目(GZ2022081)
出版年
2024
NETL
NSTL
万方数据