以單一步驟修改QuEChERS方法進行農產品中農藥殘留之快速分析

Single-Step Modified QuEChERS for Rapid Determination of Pesticide Residues in Agricultural Products

陳惠珊(Hui-Shen Chen)

指導教授 ： 郭賓崇

共同指導教授 ： 陳妙帆(Miao-Fan Chen)

國立虎尾科技大學/文理學院/生物科技研究所/碩士(2015年)

https://doi.org/10.6827/NFU.2015.00118

摘要

本研究進行玫瑰(Rosa sp.)、薰衣草(Lavandula heterophylla)、青江菜(Brassica chinensis Linn)及洋香瓜(Cucumis melo) 4種農產品中21種農藥之快速分析回收測試，使用乙腈(含1%醋酸)、無水硫酸鎂、醋酸鈉、一級二級胺吸附劑快速萃取與淨化農藥殘留，樣品混和離心後置於自動進樣瓶，以GC-MS/MS和LC-MS/MS分析之。大部分樣品基質中分別添加21種農藥之線性分析範圍(0.01-0.5 mg/L)判定係數(R2)>0.99(僅部分薰衣草、洋香瓜樣品與diflubensuron之R2未達0.995)，LOQ (Limit of quantification, S/N≥10) 範圍為0.00004-0.2 ppm (ug/g)，針對GC-MS/MS分析之10種農藥(測試濃度為0.03、0.1、0.5 μg/mL)，於玫瑰之方法回收率為90.7-122.5%（RSD：1.9-20%），於薰衣草回收率為74.8-97.5%(RSD：0.3-7.3%)，於青江菜回收率為88.5-118.1%(RSD：1.5-20%），於洋香瓜回收率為76.5-107.7%(RSD：0.3-5.4%），而LC-MS/MS分析之11種農藥(測試濃度0.03、0.1、0.5 μg/mL)於玫瑰之回收率為73.5-104.1%(RSD：0.1-13%），薰衣草回收率為65.8-131.7%(RSD：1.2-15%），青江菜回收率為81.2-123.3%(RSD：0.6-18%），洋香瓜回收率為78.7-102.9%(RSD：0.9-11%），前處理過程能縮減至20分鐘，此方法已應用在這些作物於田間實際施藥後之殘留消退分析研究。

關鍵字

農產品 ； 農藥殘留分析 ； 玫瑰 ； 薰衣草 ； 青江菜 ； 洋香瓜 ； QuEChERS

並列摘要

A rapid single-step modified QuEChERS method was developed for analysis of 21 pesticides in agricultural products, including rose (Rosa sp.), lavender (Lavandula heterophylla), Chinese mustard (Brassica chinensis Linn) and melon (Cucumis melo) samples. Fast extraction and cleanup of pesticide residues with acetonitrile containing 1% acetic acid, anhydrous magnesium sulfate, sodium acetate, and primary secondary amine sorbent were conducted at the same time. After mixing and centrifugation, the extract was transferred to autosampler vials for determination of 21 pesticide residues by GC-MS/MS and LC-MS/MS. The calibration curves were constructed from the sample matrix. The linearity of the analytical response across the studied range of concentrations (0.01-0.5 mg/L) was excellent, almost obtaining a correlation coefficient (R2) of 0.99. The limits of quantification (LOQ, S/N≥10) ranged from0.00004-0.2 ppm (ug/g). For the determination of 10 pesticides by GC-MS/MS (three levels, 0.03、0.1、0.5 μg/mL), the recoveries of pesticides were 90.7-122.5% (RSD: 1.9-20%) in roses, 74.8-97.5% (RSD: 0.3-7.3%) in lavenders, 88.5-118.1% (RSD:1.5-20%) in Chinese mustards, 76.5-107.7% (RSD: 0.3-5.4%) in melons, respectively. For the determination of 11 pesticides by LC-MS/MS, the recoveries of pesticides were 73.5-104.1% (RSD: 0.1-13%), 65.8-131.7% (RSD: 1.2-15%), 81.2-123.3% (RSD: 0.6-18%), 78.7-102.9% (RSD: 0.9-11%) in rose, lavender, Chinese muster, and melon samples, respectively. The whole procedure takes ca. 20 mins. This method has applied to study the dissipations of pesticide residues in real samples collected from fields after pesticide applications.

並列關鍵字

agricultural products ； pesticide residues ； analysis ； rose ； lavender ； Chinese mustard ； melon ； QuEChERS

參考文獻

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