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中国精品科技期刊2020
徐鹏,赵建珍,闫伟伟,等. QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中9种甲氧基丙烯酸酯类杀菌剂[J]. 食品工业科技,2021,42(7):289−295. doi: 10.13386/j.issn1002-0306.2020060021.
引用本文: 徐鹏,赵建珍,闫伟伟,等. QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中9种甲氧基丙烯酸酯类杀菌剂[J]. 食品工业科技,2021,42(7):289−295. doi: 10.13386/j.issn1002-0306.2020060021.
XU Peng, ZHAO Jianzhen, YAN Weiwei, et al. Determination of 9 Strobilurin Fungicides in Vegetables by QuECHERS-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(7): 289−295. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020060021.
Citation: XU Peng, ZHAO Jianzhen, YAN Weiwei, et al. Determination of 9 Strobilurin Fungicides in Vegetables by QuECHERS-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(7): 289−295. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020060021.

QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中9种甲氧基丙烯酸酯类杀菌剂

Determination of 9 Strobilurin Fungicides in Vegetables by QuECHERS-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了采用QuEChERS方法提取净化,超高效液相色谱-串联质谱法(UPLC/MS/MS)同时测定蔬菜中的9种甲氧基丙烯酸酯(Z-苯氧菌酯、E-苯氧菌酯、嘧菌酯、肟嘧菌胺、醚菌胺、啶氧菌酯、吡唑醚菌酯、肟菌酯、嘧螨酯)杀菌剂残留量的方法。样品经乙腈提取,采用正交试验验优选N-丙基乙二胺(PSA)和C18以及石墨化炭黑(GCB)净化用量。使用0.05%甲酸水和0.05%甲酸乙腈作为流动相梯度洗脱,目标化合物经岛津Shim-PackC18色谱柱(2.1 mm×50 mm,2 μm)分离,在正离子模式下进行测定。结果表明,9种甲氧基丙烯酸酯类杀菌剂在1~100 ng/mL范围内线性关系良好,决定系数在0.9942~0.9995之间,方法检出限(LOD)为0.05~0.3 μg/kg,定量限(LOQ)为0.2~0.9 μg/kg。在2、10和20 μg/kg三个添加水平下,五种蔬菜的回收率在77.26%~111.73%之间,相对标准偏差在0.46%~6.59%之间。该方法准确、快速、便捷、灵敏度高,能够满足蔬菜中9种甲氧基丙烯酸酯类杀菌剂的痕量检测要求。

     

    Abstract: The method was established for the nine strobilurin fungicides in vegetables by using QuEChERS method. The samples were extracted with acetonitrile and purified with n-propyl-ethylenediamine (PSA), C18 and graphitized carbon black (GCB) by orthogonal test. Using 0.05% formic acid water and 0.05%formic acid acetonitrile as mobile phase gradient elution, the target compounds were separated by Shimadzu shim pack C18 column (2.1 mm×50 mm, 2 μm) and determined in positive ion mode. The linear relationship of 9 strobilurin fungicides was good in the range of 1~100 ng/mL, the coefficient of determination was between 0.9942~0.9995. The LOD was 0.05~0.3 μg/kg and the LOQ was 0.2~0.9 μg/kg. At the levels of 2, 10 and 20 μg /kg, the recovery rates of the five vegetables were 77.26%~111.73%, and the relative standard deviation was 0.46%~6.59%. The method is accurate, rapid, convenient and sensitive, which can meet the requirements of trace detection of nine strobilurin fungicides in vegetables.

     

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