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使用液相色谱-串联质谱法评估多菌灵在茄子中的残留动态并制定收获前残留限量

Evaluation of Pencycuron Residue Dynamics in Eggplant Using LC-MS/MS and Establishment of Pre-Harvest Residue Limits.

作者信息

Lee Da-Geon, Baek Jae-Woon, Eun Hye-Ran, Lee Ye-Jin, Kim Su-Min, Min Tae-Gyu, Cho Yong-Won, Lee Yoon-Hee, Shin Yongho

机构信息

Department of Applied Bioscience, Dong-A University, Busan 49315, Republic of Korea.

出版信息

Foods. 2024 Nov 23;13(23):3754. doi: 10.3390/foods13233754.

DOI:10.3390/foods13233754
PMID:39682824
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11639895/
Abstract

Pencycuron is a fungicide whose maximum residue limit (MRL) in eggplant is either set at very low levels (0.02 mg/kg in European Union) or remains unestablished in many countries, necessitating stringent pesticide management. To enable timely interventions by farmers and regulators, pre-harvest residue limits (PHRLs) propose maximum allowable pesticide concentrations for each day during the pre-harvest period. An analytical method was developed to conduct residue determination trials, demonstrating that graphitized carbon black (GCB) effectively removes eggplant matrices during sample preparation. The LC-MS/MS method was established with a limit of quantification (LOQ) of 0.005 mg/kg, recovery rates ranging from 102.6% to 106.1% with relative standard deviation (RSD; 2.3-6.4%), and a matrix effect (%ME) of +8.1%. Residue analysis revealed a concentration of 0.045 mg/kg at 0 days after treatment (DAT), decreasing to 0.006 mg/kg at 14 DAT. The residue dynamics followed a first-order kinetic model, as confirmed by the F-test, with a rate constant of 0.1405. Therefore, the half-life was determined to be 4.9 d. Based on the MRL value of 0.02 mg/kg at 0 days before harvest (DBH), the PHRL was determined using both and , resulting in values of 0.04 mg/kg and 0.02 mg/kg at 5 days and 0.08 mg/kg and 0.03 mg/kg at 10 DBH, respectively. Using yields more conservative results, which ensures food safety under conditions of slower degradation rates.

摘要

戊菌隆是一种杀菌剂,其在茄子中的最大残留限量(MRL)在欧盟设定为极低水平(0.02毫克/千克),或在许多国家尚未确定,因此需要严格的农药管理。为了使农民和监管机构能够及时进行干预,收获前残留限量(PHRL)规定了收获前期间每天的最大允许农药浓度。开发了一种分析方法来进行残留测定试验,结果表明,在样品制备过程中,石墨化炭黑(GCB)能有效去除茄子基质。建立的液相色谱-串联质谱(LC-MS/MS)方法的定量限(LOQ)为0.005毫克/千克,回收率在102.6%至106.1%之间,相对标准偏差(RSD;2.3 - 6.4%),基质效应(%ME)为+8.1%。残留分析显示,处理后0天(DAT)时浓度为0.045毫克/千克,到14 DAT时降至0.006毫克/千克。残留动态符合一级动力学模型,经F检验确认,速率常数为0.1405。因此,半衰期确定为4.9天。根据收获前0天(DBH)时0.02毫克/千克的MRL值,使用 和 分别确定PHRL,结果在收获前5天分别为0.04毫克/千克和0.02毫克/千克,在收获前10天分别为0.08毫克/千克和0.03毫克/千克。使用 得出的结果更保守,可确保在降解速率较慢的情况下食品安全。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/048e77e660ba/foods-13-03754-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/adef0d336126/foods-13-03754-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/5d51be74329a/foods-13-03754-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/ab5b65290ffc/foods-13-03754-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/048e77e660ba/foods-13-03754-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/adef0d336126/foods-13-03754-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/5d51be74329a/foods-13-03754-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/ab5b65290ffc/foods-13-03754-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b1f/11639895/048e77e660ba/foods-13-03754-g004.jpg

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