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采用双水相体系结合高效液相色谱-串联质谱法对手性分离和测定果汁中的三唑类杀菌剂。

Enantioseparation and determination of triazole fungicides in fruit juice by aqueous biphasic system coupled with HPLC-MS/MS.

机构信息

Department of Pesticide, Plant Protection College, Shenyang Agricultural University, Shenyang, Liaoning Province, P. R. China.

出版信息

J Sep Sci. 2021 Sep;44(18):3407-3417. doi: 10.1002/jssc.202100370. Epub 2021 Jul 23.

Abstract

The aqueous biphasic system based on choline ionic liquids and ethylene/propylene oxide copolymer coupled with high-performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of the enantiomers of two fungicides: myclobutanil and tebuconazole. The influence of mass fractions of ionic liquids and the copolymer on the extraction efficiency of the target fungicides was investigated. The analytes are mainly concentrated in the bottom, copolymer-rich phase. The extraction efficiencies of the selected fungicides were significantly affected by the concentrations of the copolymer, and their extraction efficiencies decreased with the higher mass fractions of the copolymer, while the mass fraction of ionic liquids had little effect on their extraction behavior. Excellent extraction efficiency was achieved using the aqueous biphasic system based on choline L-lysinate and the copolymer. At three spiked concentrations of 0.01, 0.05, and 0.1 mg/kg, the average recoveries of the selected fungicides ranged from 80 to 89%, with the relative standard deviations in the range of 2.1-5.3%. Limits of quantitation for the enantiomers of tebuconazole and myclobutanil were 0.5 and 5.0 µg/kg, respectively. The developed system could be successfully applied to the analysis of triazole fungicides residue in real samples.

摘要

基于胆碱离子液体和环氧乙烷/环氧丙烷共聚物的双水相体系与高效液相色谱-串联质谱联用,建立了同时测定两种杀菌剂(苯醚甲环唑和戊唑醇)对映体的方法。考察了离子液体和共聚物的质量分数对目标杀菌剂萃取效率的影响。分析物主要集中在底部、富含共聚物的相中。所选杀菌剂的萃取效率受共聚物浓度的显著影响,随着共聚物质量分数的增加,其萃取效率降低,而离子液体的质量分数对其萃取行为影响较小。基于 L-赖氨酸胆碱和共聚物的双水相体系可获得优异的萃取效率。在 0.01、0.05 和 0.1 mg/kg 三个加标浓度下,所选杀菌剂的平均回收率在 80%至 89%之间,相对标准偏差在 2.1%至 5.3%范围内。戊唑醇和苯醚甲环唑对映体的定量限分别为 0.5 和 5.0 µg/kg。所建立的体系可成功应用于实际样品中三唑类杀菌剂残留的分析。

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