水產品中硝基咪唑類及其代謝物之檢驗方法開發   全文下載

Analytical Method Development for Nitroimidazoles and their Metabolites in Aquatic Products

本研究針對4種不同基質[虱目魚、土魠魚、甲魚（鱉）及蝦子]建立9項硝基咪唑類及其代謝物之檢驗方法。檢體以含1%甲酸之乙腈：甲醇（95：5, v/v）溶液及萃取粉劑（含無水硫酸鎂6 g及醋酸鈉1.5 g）進行萃取，再以乙腈飽和之正己烷進行淨化。液相層析採用Poroshell 120SB C18管柱搭配含0.1%甲酸之溶液及含0.1%甲酸之甲醇溶液作為移動相進行梯度沖提，利用串聯質譜儀配合多重反應模式進行分析。本研究參考衛生福利部食品藥物管理署公布之「食品化學檢驗方法之確效規範」於不同基質選擇3個添加濃度（0.001、0.005及0.01 ppm）進行添加回收試驗。同日內5重複之添加回收試驗結果，虱目魚之回收率為92.6-109%，土魠魚之回收率為90.7-108.4%，甲魚之回收率為91.2-105.3%，蝦肉之回收率為85.3-100.9%，同日內之變異係數均小於12%，異日間之變異係數均小於9%。9項硝基咪唑類及其代謝物之定量極限均為0.001 ppm。本方法已於112年12月26日公開，並可作為邊境查驗及後市場監測之參考。

The aim of this study was to develop a simultaneous analytical method for nine nitroimidazoles and their metabolites in 4 matrices (milk fish, Spanish mackerel, trionychidae and shrimp). The pretreatment procedure was extraction using a mixture solution of methanol and acetonitrile (5:95,v/v) containing 1% formic acid, extraction powder containing 6.0 g of anhydrous magnesium sulfate and 1.5 g of sodium acetate; followed by clean-up procedure using n-hexane saturated with acetonitrile. Chromatographic separation was achieved using a Poroshell 120SB C18 column and operated with a gradient mobile phase system consisting of methanol containing 0.1% formic acid and 0.1% formic acid in water. Analysis was performed by tandem mass spectrometry with multiple reaction monitoring (MRM) mode. The method was validated in accordance with the requirements of the validation guideline of the food chemical testing method published by TFDA. Three spiking levels at 0.001, 0.005 and 0.01μg/g were tested. The intra-day average recoveries of all analytes were in the range of 92.6-109% for milk fish, 90.7-108.4% for Spanish mackerel, 91.2-105.3% for trionychidae, and 85.3-100.9% for shrimp. The intra-day and inter-day precisions for all matrices were bellow 12% and 9%, respectively. The limits of quantification were 0.001 ppm for nine nitroimidazoles and their metabolites. The method was published on December 26, 2023 and can be used for conducting border inspection and post-market surveillance.