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在线 SFE-SFC-MS/MS 分析芒果及其果汁中吡唑醚菌酯和甲呋酰胺残留。

Online SFE-SFC-MS/MS analysis of pyraclostrobin and chiral mefentrifluconazole residues in mango and mango juice.

机构信息

Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin, China; Key Laboratory for Environmental Factors Control of Agro-product Quality Safety, Ministry of Agriculture and Rural Affairs, Tianjin, China; National Reference Laboratory for Agricultural Testing, Tianjin, China.

Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin, China; Key Laboratory for Environmental Factors Control of Agro-product Quality Safety, Ministry of Agriculture and Rural Affairs, Tianjin, China; National Reference Laboratory for Agricultural Testing, Tianjin, China.

出版信息

Food Chem. 2025 Feb 1;464(Pt 2):141731. doi: 10.1016/j.foodchem.2024.141731. Epub 2024 Oct 20.

DOI:10.1016/j.foodchem.2024.141731
PMID:39481306
Abstract

This study established an on-line SFE-SFC-MS/MS method for the determination of mefentrifluconazole (MFZ) enantiomers and pyraclostrobin (PY) in mango and mango juice. Key parameters of SFC separation and SFE extraction have been optimized for high efficiency, sensitivity, and environmental friendliness. Enthalpy controlled enantioseparations of MFZ were recognized by thermodynamic analysis. Molecular docking estimated the enantiomeric recognition of MFZ enantiomers binding to the chiral stationary phase. The mean recoveries (RSDs) were in the range of 94.5-106.8 % (4.2-15.4 %), 91.1-103 % (3.6-10.3 %), 94.7-102.7 % (3.8-9.8 %), and 93.2-106.9 % (4.1-12.1 %) for R-MFZ, S-MFZ, racemic MFZ, and PY under 3 spiked levels of interday assays (n = 15). The LOQs of R-MFZ, S-MFZ, and PY were 0.5, 0.5, and 1 μg kg. The method was further applied to real samples in Guangxi Province, China with low acute and chronic dietary risk for MFZ and PY in mango and mango juice.

摘要

本研究建立了在线 SFE-SFC-MS/MS 方法,用于测定芒果和芒果汁中的甲呋氟草醚(MFZ)对映异构体和吡唑醚菌酯(PY)。对 SFC 分离和 SFE 提取的关键参数进行了优化,以实现高效率、高灵敏度和环境友好性。通过热力学分析,对 MFZ 的热控对映体分离进行了识别。分子对接估计了 MFZ 对映体与手性固定相的对映体识别。日内测定的 3 个加标水平下,R-MFZ、S-MFZ、外消旋 MFZ 和 PY 的平均回收率(RSD)范围分别为 94.5-106.8%(4.2-15.4%)、91.1-103%(3.6-10.3%)、94.7-102.7%(3.8-9.8%)和 93.2-106.9%(4.1-12.1%)(n=15)。R-MFZ、S-MFZ 和 PY 的 LOQs 分别为 0.5、0.5 和 1μg/kg。该方法进一步应用于中国广西省的实际样品,结果表明芒果和芒果汁中的 MFZ 和 PY 具有较低的急性和慢性膳食风险。

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