液相層析串聯質譜儀分析食品中丙烯醯胺含量方法確效   全文下載

Validation of an Improved LC/MS/MS Method for Acrylamide Analysis in Foods

本研究建立一套經改善之液相層析串聯質譜儀分析方法，用以分析食品中丙烯醯胺的含量，檢體係經水萃、串聯固相萃取匣淨化及濃縮後，檢液以液相層析串聯質譜儀分析，本研究探討固相萃取匣、層析管、淨化方法及儀器最佳化條件。本方法經再現性試驗、重複性試驗及回收試驗等實驗室內確效試驗證明其可行性，並參加FAPASR 國際間實驗室精準度測試，結果符合該機構評定為滿意，顯示本方法之精確度，可作為日常分析食品中丙烯醯胺含量之標準方法。本方法之偵測極限為3 μg/kg；平均回收率介於95 至113%；重複性變異係數介於1.3 至10.0%；再現性試驗之變異係數介於3.3至6.9%。以本方法分析市售食品中丙烯醯胺含量，發現紅糖中含有丙烯醯胺，可解釋含有紅糖成分之非高溫加熱食品中亦含有丙烯醯胺之原因。

An improved LC/MS/MS method was set up and validated for analyzing acrylamide (AA ) in foods including fried potato snack food, baked breakfast food, bread, coffee and tea drinks which are the most popular stimulant drinks in Taiwan. Two types of cartridge in tandem use, elution volume, and a long column (250 mm), were used to improve the separation of interferences and reduce detection limit. Reproducibility, repeatability, and recovery tests were conducted to assure the analytical method applicable in house validation testing. Participation in the FAPAS® inter-comparison study resulted in a satisfactory result. The limit of detection was 3 μg/kg; mean recoveries ranged from 95 to 113%; coefficients of variation ranged from 1.3 to 10.0% for repeatability test and 3.3 to 6.9% for reproducibility test. The good results showed the method has been successfully set up to serve as a routinely analytical method. We also found that brown sugar with high AA contents lead to high AA content in some foods including those not cooked at high temperature.