摘要:本計畫在於建立發展全自動化農藥殘留待檢樣品的前處理工作平台,並針對農產品農藥殘毒檢驗過程建立一個全自動化之檢驗流程。本項前處理工作平台主要組成裝置包括機械手臂單元、探針自動清洗裝置、以及微波加熱單元。本計畫應用機電整合技術、精密定位自動化技術結合可程式規劃技術,對於影響微波照射功率、溫度梯度、加熱時間、攬拌設計、取樣設計、吸附時間,脫附溫度及時間等加以詳盡全自動化探討,進行研製即時人機觸控介面,以利整合農產品農藥殘留檢測時各項處理單元的參數設定與操控程序。本計畫所研發的前處理工作平台採用微波輔助頂空固相微萃取 (Microwave Assistant- Head Space-Solid Phase Microextraction, MA-HS-SPME) 技術應用於水中多種農藥分析,包括有機磷類(Organophosphates)、有機氯類(Organ chlorines)、合成除蟲菊類(Pyrethroids)、三唑類(Triazoles)及其他可電子捕獲偵測之藥劑(Others)等180種農藥,以氣相層析儀附火焰光量偵檢器(CG-FPD)及電子捕獲式偵檢器(ECD)分析。選擇DVB/CAR/PDMS_50/30 μm固相微萃取纖維管,以100 C 加熱萃取10分鐘、頂空吸附10分鐘、310 C 脫附3分鐘條件下,測試180種農藥分為9組分別添加0.1-1.0 ng在10mL水體中,頂空吸附後自動移至氣相層析儀注入口脫附並同時進入儀器,層析分析時間23分鐘內完成。以DVB/CAR/PDMS_50/30 μm纖維管而言,180種農藥中可分析141種(佔78%),其中有機磷類79種(佔72%)、有機氯類、三唑類及其他類80種(佔80%)、合成除蟲菊類21種(佔95%)。所建立之方法在水中多種農藥分析其偵測極限可達ppt,可在短時間內完成多種農藥快速篩選,每個樣品僅花40分鐘而可以檢測農藥殘留。檢測過程中無溶劑使用,屬於綠色環保分析,並且有效及準確地分析農藥殘留,極適合應用於環境水體中之多重農藥快速篩檢。本計畫成果將可取代人工式費時費力的檢測方式,建構一套快速的自動化農產品農藥殘留檢測前處理工作平台。
關鍵字:
微波輔助萃取、多種農藥同時分析、自動取樣、頂空萃取、固相微萃取、可程式規劃、機械手臂、人機界面、機電整合
Abstract: An automatic pre-processing platform for pesticide residues of agricultural produce was developed in this project. An automatic inspection procedure for pesticide residues was also established in this work. The developed pre-processing platform is mainly consisted of a robot manipulator unit, a cleaning device for inspection probe, and a microwave accelerated reaction unit. In this project, the mechatronic instrument, precisely automatic positioning technique, and programming technique were integrated to design the automatic pre-processing platform. The microwave exposure power, temperature gradient, heating time, stirring time, sampling design, absorption time, and dehydration temperature and time were taken into consideration to develop the User Graphical Interface (GUI) of the designed platform. The GUI can integrate various units used in the platform. The inspection parameters and operation procedures can also be set via GUI. The microwave assistant-head space-solid phase micro-extraction (MA-HSSPME) technique is adopted in the developed pre-processing platform. The MA-HS-SPME technique coupled with gas chromatography / electron capture detector (GC-ECD) or flame photometric detector (GC-FPD) was evaluated for the determination of 180 pesticides in water. These pesticides include organophosphates, organ chlorines, pyrethroids, triazoles, and others. The 180 pesticides were divided to 9 sets and 0.1-1.0 ng was spiked to 10 mL water in 22 mL sample vial separately. After a sample vial was heated with 100 C for 10 min, the DVB/CAR/PDMS 50/30 μm SPME fiber was selected to absorb analysts for 10 min on the head space, then desorped in 310 C for 3 min in GC inlet. The chromatography analysis will be finished in 23 min. This method performed good for 141 of 180 pesticides (78 %), involved 79 organophosphates (72 %), 80 organ chlorines, triazoles and others (80 %), 21 pyrethroids (95 %). The detection was linear in the studied concentration range with r2 > 0.9808. The detection limits varied from 0.04 to 3.34 ppb. The detection limits were determined to be in the ppt level. The proposed method provides a very simple, fast, and solvent-free procedure. The proposed method provides a very simple, fast, and solvent-free procedure. The sample pretreatment prior to the trace-level screening determination of pesticides mutli-residues by gas chromatography can be also achieved. The traditional time and labor consuming inspection method can be replaced by the developed technique so that a fast and automatic inspection for pesticide residues of agricultural produce can be achieved.
Key words:
microwave assistant extract(MAE)、multi-residue analysis、autosampler、head space extraction、solid phase microextraction (SPME)、programming、robotic arm、Graphical User Interface、mechatronics