液相色谱-高分辨飞行时间质谱法测定食品接触纸包装材料中的7种荧光增白剂  

Simultaneous Determination of Seven Fluorescent Whitening Agents in Food Contact Paper Package Materials by High Performance Liquid Chromatography Tandem Triple TOF-High Resolution Mass Spectrometry

作　　者：杜志峰[1,2,3] 冼燕萍 刘付建 郭新东 黄金凤 吴玉銮 罗海英 王永华[3] 

机构地区：[1]广州市质量监督检测研究院,广州510110 [2]爱博才思亚太应用支持中心,上海200233 [3]华南理工大学轻工与食品学院,广州510640 [4]广东产品质量监督检验研究院,广州510330

出　　处：《分析化学》2014年第5期636-642,共7页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科技计划资助项目(No.2012QK074)

摘　　要：建立了食品接触纸包装材料中7种荧光增白剂（ FWA 368, FWA 367, FWA 185, FWA 184, FWA 52, FWA 135和FWA 393）的液相色谱串联高分辨飞行时间质谱（LC-Triple TOF MS）的筛查与定量检测方法。纸质样品经三氯甲烷超声提取,浓缩,采用甲醇-0.1%甲酸为流动相,在C18色谱柱（100 mm×2.1 mm i. d.,2.6μm）上梯度洗脱分离,在电喷雾正离子及TOF MS触发TOF MS/MS的模式下检测,以保留时间、一级离子质量准确度、一级离子同位素分布、二级碎片与库匹配4种手段确保准确定性分析,以TOF MS提取离子的峰面积定量。结果表明,7种荧光增白剂的质量精确度均小于3×10-6,在4~400μg/L范围内线性关系良好,相关系数均大于0.996,仪器检出限（S/N=3）为1.0~5.0μg/kg,3个添加水平的回收率为81.2%~98.9%,相对标准偏差（n=6）为5.2%~9.1%,应用本方法检测了13个样品,其中1个样品检出含有FWA184,含量为287μg/kg。结果表明,检测方法具有高效、准确的特点,适用于食品接触纸包装材料中7种荧光增白剂含量的测定。A method for screening and quantitative detection of seven fluorescent whitening agents （ FWAs, FWA368 , FWA367 , FWA185 , FWA 184 , FWA52 , FWA135 and FWA393 ） in food contact paper package materials was established by high performance liquid chromatography tandem triple TOF high resolution mass spectrometry （ LC-Triple TOF MS） . The paper samples were extracted with chloroform under ultrasonication, concentrated, separated in a C18 column （100 mm× 2. 1 mm i. d. , 2. 6 μm） by gradient elution using methanol and 0. 1% formic acid in water as mobile phase, and detected in positive ESI and TOF-MS IDA MS/MS mode. The qualitative analysis of seven FWAs was confirmed by synergistic effect of retention time, mass accuracy of precursor, isotope distribution of the precursor, and library search. The analytes were quantified by peak areas of the TOF-MS extracted ions. The results indicated that, all of the seven FWAs presented favorable mass accuracy less than 3×10-6 , good linearity in the concentration of 4-400 μg/L with the correlation coefficients larger than 0. 996, low instrument detection limits （ S/N=3 ） of 1. 0-5. 0 μg/kg, appropriate recoveries ranged from 81. 2% to 98. 9% at three spiked levels, and satisfactory RSD （n=6） of 5 . 2% -9 . 1%. 13 samples were tested using the method and one sample was found FWA 184 with concentration of 287 μg/kg. The method is efficient and accurate, and is suitable for analysis of the seven FWAs in food contact paper package materials.

关 键 词：液相色谱-高分辨飞行时间质谱法 荧光增白剂 食品接触纸包装材料 

分 类 号：O657.63[理学—分析化学] TS206[理学—化学]