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采用快速提取方法结合超高效液相色谱-串联质谱法测定柑橘中氟吡菌酰胺和霜霉威铝的方法验证、消解和残留状况。

Method validation, dissipation and residue status of fluopicolide and fosetyl-aluminium in citrus using a rapid extraction method coupled with ultra-performance liquid chromatography-tandem mass spectrometry.

机构信息

Pesticide Residue Laboratory, Anand Agricultural University, Anand, India.

Main Forage Research Station, Anand Agricultural University, Anand, India.

出版信息

Biomed Chromatogr. 2023 Oct;37(10):e5703. doi: 10.1002/bmc.5703. Epub 2023 Jul 18.

DOI:10.1002/bmc.5703
PMID:37463672
Abstract

The dissipation and residue status of a combination of fluopicolide and fosetyl-aluminium (fosetyl-Al) in citrus were evaluated in an experimental field. An efficient and sensitive liquid chromatography-tandem mass spectrometry, with rapid extraction, was carried out according to the SANTE guidelines. During the method validation, the recovery was within the range of 106.1-117.5, 94.4-115 and 85.4-109.5%, for fluopicolide, its metabolite 2,6-dichlorobenzamide and fosetyl-Al, respectively, with a relative standard deviation (RSD) of 0.3-10.6%. As a result, accuracy and precision at the spiking concentrations of 0.01, 0.05 and 0.10 mg/kg in citrus were within the acceptable range of 70-120% with an RSD of 20%. The amount of the deposits of fluopicolide, 2,6-dichlorobenzamide and fosetyl-Al was less than the limit of quantification (LOQ) at 0.01 mg/kg at 0 day, adhering to the application in standard [1.77 + 2.66 g of active ingredient (a.i.)/L] and double (3.54 + 5.32 g a.i./L) doses. The present study proposes that the utilisation of fluopicolide and fosetyl-Al in citrus and the soil may not pose a health or environmental hazard provided that good agricultural practices are followed.

摘要

在一个实验田中评估了氟吡菌酰胺和霜脲氰(fosetyl-Al)组合在柑橘中的消解和残留情况。根据 SANTE 指南,进行了快速提取的高效灵敏液相色谱-串联质谱分析。在方法验证过程中,氟吡菌酰胺、其代谢物 2,6-二氯苯甲酰胺和霜脲氰的回收率分别在 106.1-117.5%、94.4-115%和 85.4-109.5%范围内,相对标准偏差(RSD)为 0.3-10.6%。因此,在柑橘中 0.01、0.05 和 0.10mg/kg 的添加浓度下,准确度和精密度均在 70-120%的可接受范围内,RSD 为 20%。在 0 天,氟吡菌酰胺、2,6-二氯苯甲酰胺和霜脲氰的沉积量均低于 0.01mg/kg 的定量限(LOQ),符合标准[1.77+2.66g 有效成分(a.i.)/L]和双倍(3.54+5.32g a.i./L)剂量的应用。本研究表明,只要遵循良好的农业实践,氟吡菌酰胺和霜脲氰在柑橘和土壤中的使用不会对健康或环境造成危害。

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