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噻虫啉在亚洲梨中残留的液相色谱-串联质谱确证法及其消解速率与风险评估

The disappearance rate and risk assessment of thiacloprid residues in Asian pear using liquid chromatography confirmed with tandem mass spectrometry.

作者信息

Kabir Md Humayun, Abd El-Aty A M, Rahman Md Musfiqur, Kim Sung-Woo, Choi Jeong-Heui, Lee Young-Jun, Truong Lieu T B, Lee Kang-Bong, Kim Mi-Ra, Shin Ho-Chul, Shim Jae-Han

机构信息

Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Gwangju, Republic of Korea.

Deparment of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.

出版信息

Biomed Chromatogr. 2017 May;31(5). doi: 10.1002/bmc.3861. Epub 2016 Nov 22.

DOI:10.1002/bmc.3861
PMID:27696449
Abstract

This study was undertaken to quantify the residue levels and propose the dissipation kinetics of thiacloprid formulated as suspension concentrate in field-incurred Asian pears grown under two different open-field conditions. Samples were extracted with 20% distilled water in acetonitrile; partitioned with brine water and dichloromethane; and purified with a Florisil solid phase extraction cartridge. The analyte was identified with an LC ultraviolet detector, and field-incurred samples were confirmed using LC-MS/MS. The calibration curve was linear over the range 0.05-5.0 mg/L with a satisfactory coefficient of determination (R  = 0.9994). The limits of detection and limits of quantification (LOQ) were 0.003 and 0.01 mg/kg, respectively. The recovery rate fortified to blank samples at LOQ, 10× LOQ, and the maximum residue limit (MRL) were between 73.7 and 86.2% with relative standard deviation ≤9.0%. The residual concentrations at both sites were considerably lower than the MRL (0.7 mg/kg) set by the Korean Ministry of Food Drug Safety, with biological half-lives of 5.0 and 7.4 days, for sites 1 and 2, respectively. From the pre-harvest residue limit curve, it was predicted that if the residues were <1.13 or 1.40 mg/kg 10 days before harvest, the residue level would be lower than the MRL during harvest. Risk assessment on day 0 showed an acceptable daily intake (%) of 13.0% and 11.0% for sites 1 and site 2, respectively, which indicates that the residual amounts are not hazardous to the Korean population.

摘要

本研究旨在量化两种不同露天条件下种植的亚洲梨中悬浮剂剂型噻虫啉的残留水平,并提出其消解动力学。样品用20%的乙腈水溶液萃取;用盐水和二氯甲烷进行分配;并用弗罗里硅土固相萃取柱进行净化。用液相色谱紫外检测器鉴定分析物,并用液相色谱-串联质谱法确认田间样品。校准曲线在0.05-5.0 mg/L范围内呈线性,测定系数令人满意(R = 0.9994)。检测限和定量限(LOQ)分别为0.003和0.01 mg/kg。在定量限、10倍定量限和最大残留限量(MRL)水平下对空白样品进行加标回收试验,回收率在73.7%至86.2%之间,相对标准偏差≤9.0%。两个地点的残留浓度均远低于韩国食品药品安全部设定的最大残留限量(0.7 mg/kg),第1个地点和第2个地点的生物半衰期分别为5.0天和7.4天。根据收获前残留限量曲线预测,如果收获前10天残留量<1.13或1.40 mg/kg,则收获时残留水平将低于最大残留限量。第0天的风险评估显示,第1个地点和第2个地点的可接受每日摄入量(%)分别为13.0%和11.0%,这表明残留量对韩国人群无危害。

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