Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/97742
標題: 使用UHPLC/Triple TOF 6600 系統和SWATH 數據採集技術篩選水果中農藥殘留之定量方法的開發和驗證
Development and Validation of a Quantitative Method for Screening of Pesticide Residues in Fruit using UHPLC/TripleTOF 6600 System with SWATH Acquisition
作者: 王俊彬
Jun-Bin Wang
關鍵字: 多重監測模式(MRM);SWATH採集模式;定量分析;Multiple Reaction Monitoring (MRM);SWATH acquisition;Quantitative analysis
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摘要: 
現代農業有過長的化學肥料,農藥和除草劑使用歷史,不僅使食物中的營養成分減少,各種化學殘留物甚至會損害人類健康。由於消費更多水果和蔬菜的好處,人們越來越關注農藥殘留的問題,以及對人體可能造成的影響。現今國內以衛福部食藥署於2017 年公告的「食品中殘留農藥檢驗方法-多重殘留分析方法(五)」為食品中農藥殘留的指標方法,是以多重反應監測模式(Multiple Reaction Monitoring, MRM),藉由液相層析串聯質譜儀(LC-MS/MS)及氣相層析串聯質譜儀(GC-MS/MS)共同針對373 種農藥進行專一性的監測,具有快速且準確定量等優點。由於日新月異的農藥種類不斷被開發,多重監測模式(MRM)已無法滿足上千種的農藥於同時定量分析,故本研究是以「食品中殘留農藥檢驗方法-多重殘留分析方法(五)」為基礎,利用新穎的Sequential Windowed Acquisition of all Theoretical masses (SWATH)採集技術取代傳統的多重監測模式(MRM),以液相層析串聯質譜儀(LC-MS/MS)針對293 種農藥於同時定量分析之研究,SWATH 採集技術可收集樣品中完整的離子碎片,並加以定量分析,並可在一次樣品分析中,解決可能因樣品基質干擾產生的問題。以293 種農藥進行分析方法確效,評估方法的準確度、精密度、再現性等,在批次內精密度與準確度測試之準確度合格率為100%,精密度合格率為97.61%;批次間精密度測試之精密度合格率為98.63%;91.81%的農藥提取回收率介於70 ~ 120%之間;偵測極限(LOD)與定量極限(LOQ)測試中皆符合「食品中殘留農藥檢驗方法-多重殘留分析方法(五)」對蔬果定量極限為0.01 ppm 之要求。盲樣測試中17 種農藥皆通過測試標準。本研究透過TripleTOF 6600 質譜儀搭配SWATH 採集模式具有高準確度、高解析度及掃描速度快等優點,可作為未來農藥定量分析之平台。

The modern agriculture has a long history of chemical fertilizers, pesticides and herbicides, which not only reduces the nutrients in food, but also damages human health. Due to the benefits of consuming more fruits and vegetables, people are increasingly concerned about the problem of pesticide residues and the possible impact on the human body. Nowadays, the 'Test Method for Residual Pesticides in Foods - Multiple Residue Analysis Method (V)' announced by the Food and Drug Administration of Taiwan in 2017 is the indicator method for pesticide residues in food. It is based on multiple reaction monitoring (MRM), liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography tandem mass spectrometry (GC-MS/MS) are used to monitor the 373 pesticides, which has the advantages of high specificity, rapid and accurate quantification. As the variety of pesticides is constantly being developed, multiple reaction monitoring (MRM) have been unable to meet the quantitative analysis of more than a thousand pesticides at the same time. Therefore, this study based on the 'Test Method for Residual Pesticides in Foods - Multiple Residue Analysis Method (V)' uses the novel Sequential Windowed Acquisition of all Theoretical masses (SWATH) acquisition technology to replace the traditional multiple reaction monitoring (MRM). Liquid chromatography tandem mass spectrometry (LC-MS/MS) are used for the simultaneous quantitative analysis of 293 pesticides. SWATH acquisition technology collects intact ion fragments and quantifies from a sample, It can resolve problems that may be caused by sample matrix interference in a single sample analysis. The analytical method was validated with 293 pesticides, and the accuracy, precision, and reproducibility of the method III were evaluated. The result of precision and accuracy test, the pass rate of accuracy test is 97.61%; the pass rate of precision test is 98.63%; 91.81% of pesticides extraction recovery rate between 70 and 120%; the test of the limit of quantitation (LOQ) are in compliance with the 'Test Method for Residual Pesticides in Foods -Multiple Residue Analysis Method (V)' requirement for a vegetable and fruit of 0.01ppm. All of the 17 pesticides in the blind test passed the test criteria. In this study, the TripleTOF 6600 mass spectrometer with SWATH acquisition mode has the advantages of high accuracy, high resolution and fast scanning speed, which can be used as a platform for quantitative analysis of pesticides in the future.
URI: http://hdl.handle.net/11455/97742
Rights: 同意授權瀏覽/列印電子全文服務,2021-08-31起公開。
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