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超高效液相色谱-串联质谱法同时测定植物源食品中两种琥珀酸脱氢酶抑制剂类杀菌剂的对映体。

Simultaneous enantioselective determination of two succinate- dehydrogenase-inhibitor fungicides in plant-origin foods by ultra-high performance liquid chromatography-tandem mass spectrometry.

机构信息

Citrus Research Institute, Southwest University, Chongqing 400712, China; Laboratory of Citrus Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture and Rural Affairs, Chongqing 400712, China; National Citrus Engineering Research Center, Chongqing 400712, China.

Citrus Research Institute, Southwest University, Chongqing 400712, China; Laboratory of Citrus Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture and Rural Affairs, Chongqing 400712, China; National Citrus Engineering Research Center, Chongqing 400712, China.

出版信息

J Chromatogr A. 2022 Aug 16;1677:463325. doi: 10.1016/j.chroma.2022.463325. Epub 2022 Jul 10.

DOI:10.1016/j.chroma.2022.463325
PMID:35853420
Abstract

Fluindapyr and penthiopyrad are two new succinate-dehydrogenase-inhibitor fungicides both employed as racemic mixtures of enantiomers to control various fungal pathogens. In the present work, a robust and highly-sensitive method for simultaneous determination of fluindapyr and penthiopyrad enantiomers in plant-origin foods (cereals, fruits and vegetables) was developed using UPLC-MS/MS combined with a chiral stationary phase. Rapid baseline chiral separation of four stereoisomers of fluindapyr and penthiopyrad was obtained within 4.2 min on chiral MX(2)-RH column under reversed-phase conditions (with the eluent of acetonitrile/0.1% formic acid in water =70/30 (V:V) and column temperature maintained at 30 °C). The plant-origin samples were extracted quickly with acetonitrile and purified with multi-walled carbon nanotubes. Excellent linearity for the target analytes was observed in the concentration ranging from 1 to 250 µg/L with regression coefficient no less than 0.9967. The mean recoveries of fluindapyr and penthiopyrad enantiomers from six matrices were 77.1-107.2%, with all relative standard deviations values lower than 9.1%. The limit of quantification of four stereoisomers of two target chiral fungicides was 5 µg/kg. The analysis of real samples reveal that the developed method is suitable for the simultaneous chiral determination of fluindapyr and penthiopyrad residues in cereals, fruits and vegetables samples at enantiomeric level and can support their further investigation on enantioselective environmental behaviors and residue surveillance.

摘要

氟啶吡菌胺和戊吡菌酮是两种新型琥珀酸脱氢酶抑制剂杀菌剂,均以对映异构体的外消旋混合物形式用于控制各种真菌病原体。本研究采用超高效液相色谱-串联质谱联用手性固定相建立了一种同时测定植物源食品(谷物、水果和蔬菜)中氟啶吡菌胺和戊吡菌酮对映异构体的灵敏方法。在反相条件下(流动相为乙腈/0.1%甲酸水溶液=70/30(V:V),柱温保持在 30°C),在 MX(2)-RH 手性柱上,四种立体异构体的氟啶吡菌胺和戊吡菌酮可在 4.2 min 内快速基线分离。植物源样品用乙腈快速提取,用多壁碳纳米管净化。目标分析物在 1 至 250 µg/L 的浓度范围内具有良好的线性关系,相关系数不低于 0.9967。氟啶吡菌胺和戊吡菌酮对映异构体在六种基质中的平均回收率为 77.1-107.2%,所有相对标准偏差值均低于 9.1%。两种目标手性杀菌剂的四个立体异构体的定量限均为 5 µg/kg。实际样品分析表明,该方法适用于谷物、水果和蔬菜样品中氟啶吡菌胺和戊吡菌酮残留的同时对映体测定,可支持进一步研究其对映选择性环境行为和残留监测。

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