QuEChERS-高效液相色谱-串联质谱法同时测定陈皮中多种杀菌剂
Simultaneous detection of multiple fungicides in Citri Reticulatae Pericarpium with QuEChERS-high performance liquid chromatography-tandem mass spectrometry
投稿时间:2021-06-04  修订日期:2021-08-25
DOI:
中文关键词:  QuEChERS  高效液相色谱-串联质谱法  陈皮  杀菌剂
英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  Citri Reticulatae Pericarpium  fungicides
基金项目:
作者单位
胡晓霞 江门市农业环境监测站 
黄子亮 江门市农业环境监测站 
杨家迪 江门市农业环境监测站 
黄永东 广东省农业科学院 
AuthorInstitution
Hu Xiao-Xia Jiangmen Agricultural Environment Monitoring Station 
Huang Zi-Liang Jiangmen Agricultural Environment Monitoring Station 
Yang Jia-Di Jiangmen Agricultural Environment Monitoring Station 
Huang Yong-Dong Guangdong Academy of Agricultural Sciences,Institute of Quality and Monitoring Technology for Agro-products 
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中文摘要:
      目的 建立QuEChERS-高效液相色谱-串联质谱法(QuEChERS-high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时测定陈皮中11种杀菌剂。方法 采用QuEChERS法作为前处理方法,通过添加适量的石墨化炭黑(graphitized carbon black, GCB)和C18优化QuEChERS填充料组分,并采取0.1%甲酸水-甲醇作为流动相进行梯度洗脱,用基质匹配外标法对陈皮中11种杀菌剂进行定量分析。结果 优化的QuEChERS法对11种杀菌剂的基质效应系数均小于10%。并且,通过优化液相条件和多重反应监测(MRM)下的质谱参数,11种杀菌剂可以很好地分离并实现较好的灵敏度,检出限范围为0.07?0.19 μg/kg,线性关系良好(R2>0.993),平均加标回收率为75?95%,相对标准偏差RSD均小于10%。结论 该研究方法高效、快速、灵敏,精密度能达到定量分析要求,能够为陈品样品中杀菌剂类农药残留的快速筛查提供可靠的技术支持,可有效提升陈皮市场的安全性。
英文摘要:
      Objective To develop a multi-residue analysis method depending on QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the determination of 11 kinds of fungicides in Citri Reticulatae Pericarpium. Methods QuEChERS technique was used as the pre-treatment method. The filling material was optimized by adding appropriate amounts of graphitized carbon black (GCB) and C18, and the gradient elution was carried out with 0.1% formic acid and acetonitrile as mobile phase. The matrix matching external standard method was applied to quantify. Results The optimized QuEChERS method exhibits weaker matrix effect, and the matrix effect coefficients for the 11 fungicides are all less than 10%. Additionally, under the multiple reaction monitoring (MRM) mode, the liquid conditions and mass spectrometry parameters were optimized, achieving good separation and sensitivity. The limits of detection (LODs, S/N = 3) of this method were between 0.07-0.19 μg/kg. 11 kinds of fungicides showed good linear relationship (R2>0.993). The average recoveries of the 11kinds of fungicides in Citri Reticulatae Pericarpium were between 75% and 95%. The relative standard deviations (RSDs) were less than 10%. Conclusion Our developed method is efficient, fast, and sensitive, and the precision can meet the requirements of quantitative analysis. It can provide reliable technical support for the rapid screening of fungicide pesticide residues in Citri Reticulatae Pericarpium, and can effectively improve the safety of the Citri Reticulatae Pericarpium market.
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