高效液相層析串聯質譜法分析食品中之防腐劑

Determination of Preservatives in Foods by Liquid Chromatography/Tandem Mass Spectrometry

蔡佳芬(Chia-Fen Tsai) ； 郭景豪(Ching-Hao Kuo) ； 黃立宇(Li-Yu Huang) ； 曾素香(Su-Hsiang Tseng) ； 蘇淑珠(Shu-Chu Su) ； 闕麗卿(Lih-Ching Chiueh)

《食品藥物研究年報》 2期 (2011/12) Pp. 97-106

https://doi.org/10.6945/ARFDR.201112.0099

摘要

本研究建立以高效液相層析串聯質譜法（liquid chromatography/tandem mass spectrometry，LC/MS/MS）利用負離子電灑法以多重反應偵測（multiple reaction monitoring，MRM）模式同時檢測食品中苯甲酸(benzoic acid)、對羥苯甲酸（p-hydroxy-benzoic acid）、水楊酸（salicylic acid）、對羥苯甲酸甲酯（methyl p-hydroxybenzoate）、對羥苯甲酸乙酯（ethyl p-hydroxybenzoate）及對羥苯甲酸丙酯（propyl p-hydroxybenzoate）、對羥苯甲酸異丙酯（isopropyl p-hydroxybenzoate）、對羥苯甲酸丁酯（butyl p-hydroxybenzoate）、對羥苯甲酸異丁酯（isobutyl p-hydroxybenzoate）及對羥苯甲酸間丁酯（sec-butyl p-hydroxybenzoate) 10項防腐劑之檢驗方法。精確量取檢體5g加水與甲醇（1:1，v／v）溶液30mL，振盪30分鐘，以去離子水定容至50mL，混勻，於4000 rpm離心10分鐘，取上清液經0.22μm濾膜過濾後，使用Agilent Poroshell 120 EC-C18（2.7μm，4.6×100mm）層析管柱，以0.1%甲酸溶液與含0.1%甲酸之甲醇為移動相進行梯度流洗，再以串聯質譜儀分析。泡麵類食品添加防腐劑混合標準溶液，使其添加濃度為0.01、0.02、0.04g／kg，行三重複試驗，回收率介於60－115%，變異係數小於20%。

關鍵字

高效液相層析串聯質譜法 ； 防腐劑

並列摘要

A method for the analysis of 10 preservatives in foods by liquid chromatography/tandem mass spectrometry (LC/MS/MS) with electrospray ionization was developed. Data acquisition under MS/ MS for every preservative was achieved by applying multiple reaction monitoring (MRM). Benzoic acid, p-hydroxy-benzoic acid, salicylic acid, methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, propyl p-hydroxybenzoate, isopropyl p-hydroxybenzoate, butyl p-hydroxybenzoate, isobutyl p-hydroxybenzoate and sec-butyl p-hydroxybenzoate were extracted from foods with 50% methanol (v/v), and analyzed by LC/MS/MS with electrospray ionization. The LC separation was conducted on an Agilent Poroshell 120 EC-C18 (2.7 μm, 4.6 × 100 mm) column with gradient elution of 0.1% formic acid in water and methanol as the mobile phase. The recoveries of 10 preservatives (0.01, 0.02 and 0.04 g/kg) spiked in instant noodles ranged from 60 to 115% and the coefficients of variation of all preservatives were below 20%.

並列關鍵字

liquid chromatography/tandem mass spectrometry ； preservatives