表面增強拉曼散射(surface-enhanced Raman scattering, SERS)透過分子振動產生散射光譜指紋，能提供識別功能，極具潛力作為生物醫學、環境污染及食品安全之篩檢工具。本研究以斜向沉積技術(glancing angle deposition, GLAD)製備奈米銀顆粒(Ag nanoparticles, AgNPs)和奈米銀合金(Ag@Au)陣列結構之SERS基底，並開發偵測農作物中微量農藥殘留之基質淨化程序，應用於分析萃取液成分及確效，評估利用表面增強拉曼光譜分析農藥殘留之適用性。
本研究針對國內農作物栽種常使用的除草劑巴拉刈(paraquat, PQ)和殺菌劑二硫代胺基甲酸鹽(dithiocarbamates, DTCs)進行偵測，由於PQ分子極性高而難以利用吸收劑淨化，DTCs受限於分子結構而難以質譜儀定性，因此無法依照標準多重農藥殘留分析方法製備檢液。PQ在許多國家普遍用來控制田園雜草，產生自由基造成細胞組織不可逆傷害及器官壞死，國內於2020年禁止PQ使用，但礙於公告檢驗方法流程繁瑣且需LC/MSMS進行精確定量，不利田間監測和機動查緝。因此，本研究使用歐盟QuPPe萃取方式，建立AgNPs-SERS基底快速篩檢紅豆中PQ殘留之分析最適條件，其偵測PQ極限達0.8 ng/g。
此外，DTCs是國內使用量大且用途廣泛的殺菌劑農藥，其毒性差異由分子結構決定，大致上可歸類為三種分子結構dimethyldithiocarbamates (DMDCs)、ethylene-bis-dithiocarbamates (EBDCs)及propylene-bis-dithiocarbamates (PBDCs)，其中EBDCs和PBDCs的代謝物具有不同毒性。現行國內外公告DTCs檢驗方法為經由還原劑測定二硫化碳總量，易受作物內生性硫化物干擾造成偽陽性且無法鑑別DTC種類。對此，本研究開發Ag@Au-SERS基底檢測蔬果基質中DTCs種類和殘留量，其偵測極限達0.05 μg/g，對於內源性硫化物含量高的作物(如花椰菜和白蘿蔔)，無基質干擾效應。應用低濃度DTCs殘留的萵苣樣品所作的篩檢效能統計，靈敏度達93.3%以上，偽陰性低於6.7%。進一步藉由基線校正圖譜，透過機器學習訓練辨識模組，採用單一層級支持向量演算函式(One Calss SVM)，強化對偽陰性結果的辨識。
本論文研究成功利用奈米結構SERS基底建立可快速偵測作物基質中PQ和DTCs殘留之分析方法。此分析方法具有操作簡單、排碳量低、安全性高、無基質干擾等優點，可與現行公告檢驗方法互補，提供快速篩檢或自主管理之使用。

Surface-enhanced Raman scattering (SERS) generates scattering spectral fingerprints through molecular vibrations, which can provide identification functions and have great potential as a screening tool for biomedicine, environmental pollution and food safety. This study developed SERS substrates with the array structure of Ag nanoparticles (AgNPs) and Ag@Au by glancing angle deposition (GLAD) and a substrate purification procedure for detecting trace pesticide residues in crops, and evaluated the validity of SERS performance for the analysis of pesticide residues.
In this study, the herbicide paraquat (PQ) and the fungicide dithiocarbamates (DTCs) commonly applied in domestic crop cultivation. The standard multiplex pesticide residue analysis methods can not be used because the high polarity of PQ molecules is difficult to purify by absorbents, and the molecular structure of DTCs is difficult to characterize by mass spectrometry. PQ is commonly used in many countries to control weeds in fields, which generate free radicals that can cause irreversible cell tissue damage and organ necrosis. Thus, this study established the optimal conditions for the rapid screening of PQ residues in red beans using the EU QuPPe extraction method with AgNPs-SERS substrate, and the detection limit of PQ reached 0.8 ng/g.
In addition, DTCs are widely used fungicidal pesticides, and their toxicity differences are determined by their molecular structures, which can be roughly divided into three types of molecular structures： dimethyldithiocarbamates (DMDCs), ethylene-bis-dithiocarbamates (EBDCs) and propylene-bis-dithiocarbamates (PBDCs). The metabolites of EBDCs and PBDCs have different toxicity. At present, the determination method of DTCs are based on the determination of total carbon disulfide by reducing agents, which are susceptible to the interference of endogenous sulfides in crops, resulting in false positives and unidentifiable DTC species. This study developed Ag@Au-SERS substrates to detect DTCs species and residues in vegetable and fruit matrices with a detection limit of 0.05 μg/g for crops with high endogenous sulfide content (e.g., cauliflower), and there was no matrix interference effect.
This study successfully developed a rapid detection method for PQ and DTCs residues in crop matrices using nanostructured SERS substrates. This analytical method has the advantages of simple operation, low carbon emission, high safety, and no matrix interference, which can be complementary to the current announcementinspection assays to provide rapid screening or self-management.

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