膠囊錠狀食品中檸檬酸三乙酯檢驗方法之建立

Determination of Triethyl Citrate in Foods in Capsule or Tablet form

檸檬酸三乙酯為我國准用之食品添加物，列屬品質改良用、釀造用及食品製造用劑，依食品添加物使用範圍及限量暨規格標準之規定可使用於膠囊與錠狀食品，限量為3.5 g／kg。本研究建立以氣相層析串聯質譜儀進行膠囊與錠狀食品中檸檬酸三乙酯之檢驗方法，將檢體均質混勻，取約1g，精確稱定，置於25mL容量瓶中，加入10μg／mL 1,1,2-乙烷三羧酸三乙酯內部標準溶液1.25mL及正己烷20mL，超音波振盪10分鐘，以正己烷定容，經濾膜過濾，供作檢液。於空白檢體中添加適當檸檬酸三乙酯標準溶液，使成為0.25及1.25mg／kg之添加量，進行回收率及重複性試驗。實驗結果檸檬酸三乙酯於0.25及1.25mg／kg之回收率分別為112.4及103.6％，變異係數分別為3.47及4.29％，顯示方法之回收率良好、再現性高，本檢驗方法之定量極限為0.25mg／kg，並已公開為建議檢驗方法供各界參考引用。利用本方法進行11件市售膠囊與錠狀食品之檸檬酸三乙酯分析，結果顯示有1件與標示不符，經後續追查係來自添加之香料所帶入。 Triethyl citrate is a legal food additive. It is added to food in capsule or tablet form as an agent for quality improvement, distillery and food processing. An analytical method for the determination of triethyl citrate in food in capsule or tablet form by gas chromatography coupled with tandem mass spectrometry (GC/MS/MS) was developed. The recovery tests were carried by spiking standards into blank samples. The results showed great linearity of calibration. The recoveries of triethyl citrate were between 112.4 and 103.6% with coefficients of variation (CV) between 3.47 and 4.29% at 0.25 and 1.25 mg/kg, respectively. The quantification limit of triethyl citrate was 0.25 mg/kg. This method was employed in testing 11 commercial products. One sample was found not in compliance of labeling inspection with regulations due to the added spice.