食品中溴酸鹽檢驗方法之建立   全文下載

Development of an Analytical Method for Bromate in Foods

溴酸鉀曾為我國准用之食品添加物，可使用於麵粉中作為麵粉改良劑，但世界衛生組織於1986年公布其有致癌之潛在危害，並將其從食品添加物列表中移除，我國亦於1994年公告禁用。因應在2007年國外有於洋芋片中檢測出溴酸鉀之相關新聞報導，本研究建立以超高效液相層析串聯式質譜儀（Ultra Performance Liquid Chromatograph-tandem Mass Spectrometer, UPLC-MS/MS）檢測食品中溴酸鹽之檢驗方法。檢體以70%乙腈溶液萃取，經固相萃取匣淨化後以UPLC-MS/MS分析，使用BEH Amide之層析管柱（1.7μm, 2.1 mm × 10 cm），搭配50 mM甲酸銨溶液及乙腈進行梯度沖提。確效結果顯示，以麵粉作為基質，添加50及500 ng/g溴酸鹽之同日內平均回收率分別為105.3及108.3%，變異係數為10.3及6.9%，異日間變異係數為8.8%及9.8%；以洋芋片作為基質之同日內平均回收率為114.6及114.7%，變異係數為8.7及5.7%，異日間變異係數為7.3%及4.7%；本方法之定量極限為50 ng/g。以所建立之分析方法應用於市售11件相關食品檢體檢驗，結果皆為未檢出溴酸鹽。

An analytical method for determining bromate in foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Sample was extracted with 70% acetonitrile solution, further clean-up was achieved with solid-phase extraction, and then the extract was analyzed by UPLC-MS/MS. The separation was conducted on a BEH Amide column with 50 mM aqueous ammonium formate acetonitrile mobile phase by a gradient program. The recovery, repeatability and limit of quantification studies were evaluated by spiking bromate standards into the blank samples at the level of 50 and 500 ng/g. In flour matrix, the average recoveries of bromate were 105.3% and 108.3%, the coefficients of variation were 10.3% and 6.9%, repestively. The intraday and interday coefficients of variation were obtained 8.8% and 9.8%, respectively. In potato chip matrix, the average recoveries of bromate were 114.6% and 114.7%, the coefficients of variation were 8.7% and 5.7%, repestively. The intraday and interday coefficients of variation were obtained 7.3% and 4.7%, respectively. The limit of quantification was 50 ng/g. This analytical method was further applied to 11 related samples, and bromate was not detected in those samples.