CAJ | 학술논문

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。
건립료식품접촉지포장재료중7충형광증백제( FWA 368, FWA 367, FWA 185, FWA 184, FWA 52, FWA 135화FWA 393)적액상색보천련고분변비행시간질보(LC-Triple TOF MS)적사사여정량검측방법。지질양품경삼록갑완초성제취,농축,채용갑순-0.1%갑산위류동상,재C18색보주(100 mm×2.1 mm i. d.,2.6μm)상제도세탈분리,재전분무정리자급TOF MS촉발TOF MS/MS적모식하검측,이보류시간、일급리자질량준학도、일급리자동위소분포、이급쇄편여고필배4충수단학보준학정성분석,이TOF MS제취리자적봉면적정량。결과표명,7충형광증백제적질량정학도균소우3×10-6,재4~400μg/L범위내선성관계량호,상관계수균대우0.996,의기검출한(S/N=3)위1.0~5.0μg/kg,3개첨가수평적회수솔위81.2%~98.9%,상대표준편차(n=6)위5.2%~9.1%,응용본방법검측료13개양품,기중1개양품검출함유FWA184,함량위287μg/kg。결과표명,검측방법구유고효、준학적특점,괄용우식품접촉지포장재료중7충형광증백제함량적측정。
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 mmí 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 3í10-6 , 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.