比較電灑游離法與大氣壓化學游離法結合液相層析串聯式質譜儀對農藥檢測之差異

Comparison of electrospray ionization and atmospheric-pressure chemical ionization in pesticide analysis using LC-MS/MS

蔣沛廷(Chiang Pei-Ting)

指導教授 ： 陳頌方

國立臺灣師範大學/理學院/化學系/碩士(2021年)

https://doi.org/10.6345/NTNU202100340

摘要

農藥的使用使人類文明蓬勃發展，其帶來的效益讓作物能夠穩定生長並提供我們足夠的食物。但隨著農藥的用量越來越多，對環境跟人體的會造成不同程度的毒性影響身體健康甚至生命安全。依據2017年我國衛生福利部食品藥物管理署的規範，食品中殘留農藥的檢測方法訂定了373項，利用液相層析串聯質譜儀搭配電灑游離法和氣相層析串聯質譜儀搭配電子游離法進行分析。本實驗利用液相層析串聯式質譜儀的技術針對現行農藥殘留公告方法中農藥進行實驗，移動相使用甲酸銨水溶液搭配甲醇，比較大氣壓化學游離法與電灑游離法對於各農藥之游離效率。原以電灑游離法分析之196項農藥中，有6項農藥在大氣壓化學游離法下有比電灑游離法更佳的靈敏度；原以電子游離法分析之177項農藥中找出43項化合物以大氣壓化學游離法配合液相層析質譜法進行分析，並能夠符合現行法規之定量極限。結果顯示大氣壓化學游離法對擁有Triazine、Imidazole、Triazole、Pyrazole等官能基之農藥游離效率極佳。線性範圍落在1 - 200 ng/mL之間，相關係數皆在r = 0.996以上；準確度介於 86.7% - 138.8%；精密度使用變異係數表示數值介於0.19% - 13.87%。

關鍵字

農藥 ； 大氣壓游離法 ； 液相層析-串聯式質譜儀 ； 定量

並列摘要

The use of pesticides has made human civilization to flourish, and its benefits have allowed crops to grow steadily and provide us with sufficient food. However, the increasing use of pesticides let the environment and the human body expose to different levels of toxicity, which affects health even life safety. According to the regulation of the Taiwan Food and Drug Administration (TFDA) in 2017, there are 373 pesticides detection with the test methodfor pesticide residues in food, which are analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) and gas chromatography tandem mass spectrometry (GC-MS/MS) with electron ionization (EI). In this study, the pesticides were separated using an aqueous solution of ammonium formate with methanol as the mobile phase, and ionization efficiency comparison was made between atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI). Among the 196 pesticides originally analyzed by the ESI method, 6 pesticides had better peak areas and better signal-to-noise ratios using APCI; 43 pesticides originally analyzed by the EI method, and good analytical results were also obtained by APCI method.. Among them, the APCI method provided superior efficiency for pesticides which had Triazine, Imidazole, Triazole, Pyrazole functional groups. The linear range was from 1 to 200 ng/mL, and the coefficient of determination were all above r = 0.996. The accuracy ranged from 81.8% to 138.8%, and the precision was between 0.19% and 13.87%.

並列關鍵字

Pesticides ； Atmospheric pressure chemical ionization ； LC-MS/MS ； Quantification

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