- 期刊
串聯質譜儀於食用油中銅葉綠素鑑別確效與應用
Method Validation and Applications for the Identification Test of Copper(II) Chlorophylls in Edible Oils Using Tandem Mass Spectrometry
摘要
銅葉綠素為一組油溶性葉綠素之金屬錯合物（metallo-chlorophyll complexes）。本研究係依據食品藥物管理署（TFDA）公布以液相層析串聯質譜儀（LC/MS/MS）方法，進行食用油中銅葉綠素鑑別試驗之檢驗技術探討。鑑別程序包括樣品前處理，利用Silica固相萃取管（SPE）進行純化，最後再以液相層析串聯質譜儀（LC/MS/MS）大氣壓化學游離法負離子模式（atmospheric pressure chemicalionization negative mode，APCI-）之多重反應監測（multiple reaction monitoring，MRM）進行分析。供試的四組MRM離子對分別是873.6/522.1、873.6/550.1、873.6/594.1與873.6/535.1。經由確效試驗、TFDA盲樣與市售商品（葵花油、芥花油及橄欖油）分析結果，顯示QC樣品HPLC滯留時間為10.96±0.03 min （0.24%, n = 3），及m/z535.1/550.1、m/z 552.1/550.1與m/z594.1/550.1之相對離子強度（n = 3），分別是7.90± 0.94（11.91%）、56.95±0.42（0.73%）與76.85± 0.32（0.41%），均能符合鑑別允收標準（acceptance criteria）。至於空白橄欖油樣品添加試驗，顯示方法最佳偵測極限（S/N = 3）可達1 g/g。證明食品藥物管理署公布的銅葉綠素鑑別方法具有良好專一性、精密度、靈敏度及適用性。
並列摘要
Copper(II) chlorophylls is a hydrophobic mixture consisting of metallo-chlorophyll complexes. Method validation for the identification test of copper(II) chlorophylls in edible oils was achieved in accordance with the recently released method by Food and Drug Administration, Ministry of Health and Welfare, Taiwan (TFDA). Edible oils were dissolved and purified by Solid- Phase Extraction (SPE) tubes before analysis by high performance liquid chromatography-at-mospheric pressure chemical ionization-tandem mass spectrometry (LC/APCI/MS/MS) in negative mode. Four multiple reaction monitoring (MRM) transitions, i.e. 873.6/522.1, 873.6/550.1, 873.6/594.1, and 873.6/535.1 were carried out. Quality control (QC) samples, blind samples provided by TFDA and commercial edible oil (sunflower oil, canola oil and olive oil) were analyzed by the proposed methods. The analyte with the retention time of 10.96 ± 0.03 min (0.24%, n = 3) was identified to be Cu-pyropheophytin a. The average relative product ion (RPI) intensities (n = 3) of m/z 535.1 to m/z 550.1, m/z 552.1 to m/z 550.1, and m/z 594.1 to m/z 550.1 were found of 7.90 ± 0.94 (11.91%), 56.95 ± 0.42 (0.73%), and 76.85 ± 0.32 (0.41%), respectively. Limit of detection (LOD), determined at signal to noise (S/N) ratios of 3, was 1 g/g. In summary, validation parameter, including specificity, precision, and LOD, indicated the identification method promulgated by TFDA is acceptable for its intended purpose.