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基质敏感气相色谱法分析红辣椒中的吡虫清:消解模式和 PHRL 的应用。

A matrix sensitive gas chromatography method for the analysis of pymetrozine in red pepper: application to dissipation pattern and PHRL.

机构信息

Natural Products Chemistry Laboratory, Biotechnology Research Institute, Chonnam National University, Gwangju 500-757, Republic of Korea.

出版信息

Food Chem. 2014 Mar 1;146:448-54. doi: 10.1016/j.foodchem.2013.09.052. Epub 2013 Sep 18.

Abstract

A gas chromatography (GC) method for the analysis of pymetrozine was developed after utilizing matrix enhancement effect of pymetrozine to nitrogen phosphorus detector (NPD). Samples were extracted with acetonitrile and purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix-matched calibration curve prepared after spiking standard pymetrozine across the studied range of concentrations (0.003-1.0mg/L) into blank red pepper extract was excellent with a determination coefficients (R(2))=1. Recovery studies were carried out at three concentration levels (0.04, 0.4, and 2.0mg/kg, n=3) and the rates were ranged between 77.2% and 109.1%, with relative standard deviations ranged from 1.3% to 16.4%. The developed method was applied to field samples to characterize the dissipation pattern, half life, and pre-harvest residue limits (PHRL). The dissipation rates of the analyte were ascribed to first-order kinetics with half-life of 2.7 and 2.5days for recommended and double the recommended doses. From the PHRL curve, we could predict that if the residue level of pymetrozine is below the 1.23mg/kg at 10days or 0.71mg/kg at 7days before harvest, then the residues will be below the maximum residue limits (MRL=0.2mg/kg) established by the Korea Food and Drug Administration (KFDA).

摘要

建立了一种利用吡虫脒对氮磷检测器(NPD)的基质增强效应来分析吡虫脒的气相色谱(GC)方法。样品用乙腈提取,通过初级/次级胺(PSA)和 C18 分散性吸附剂进行净化。将标准吡虫脒在研究浓度范围内(0.003-1.0mg/L)加入空白红辣椒提取物中进行基质匹配校准曲线的制备,效果很好,决定系数(R²)=1。在三个浓度水平(0.04、0.4 和 2.0mg/kg,n=3)进行了回收率研究,回收率在 77.2%至 109.1%之间,相对标准偏差在 1.3%至 16.4%之间。该方法应用于田间样品,以表征消解模式、半衰期和采收前残留限量(PHRL)。分析物的消解速率归因于一级动力学,推荐剂量和推荐剂量的两倍的半衰期分别为 2.7 和 2.5 天。从 PHRL 曲线可以预测,如果吡虫脒的残留水平在 10 天或 7 天收获前低于 1.23mg/kg 或 0.71mg/kg,则残留量将低于韩国食品药品管理局(KFDA)规定的最大残留限量(MRL=0.2mg/kg)。

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