食品多组分添加剂及非法添加物的HPLC—HRMS广谱筛查
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(1. 长沙环境保护职业技术学院,湖南 长沙 410004;2. 湖南省检验检疫科学技术研究院,湖南 长沙 410004;3. 湖南出入境检验检疫局,湖南 长沙 410004)

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张帆,女,长沙环境保护职业技术学院讲师,博士。

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“十二五”国家科技支撑计划课题资助(编号:2012BAK08B01);粮油深加工与品质控制湖南省2011协同创新项目资助


Wide-scope screening of multiple and illegal additives in foods by high performance liquid chromatography-high resolution mass spectrometry
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(1. Changsha Environmental Protection College, Changsha, Hunan 410004, China; 2. Hunan Academy of Science and Technology for Inspection and Quarantine, Changsha, Hunan 410004, China; 3. Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha, Hunan 410004, China)

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    摘要:

    采用离子阱飞行时间串联质谱(LCMS-IT-TOF) 技术对葡萄酒、果汁等饮料中多组分添加剂和禁用染料进行快速筛查和确证。构建了合成色素、甜味剂、禁用染料等41种化合物的精确分子质量数和多级质谱碎片离子数据库。样品经甲醇—水(体积比11)稀释后,以C18色谱柱(150 mm × 4.6 mm,5 μm)分离,甲醇和2 mmol/L乙酸铵为流动相梯度洗脱。筛查检出限为0.005~1.000 mg/kg。在3个添加浓度下平均回收率41.2%~114.1%,相对标准偏差(RSD) 为4.3%~16.4%。利用精确质量数和数据库中质谱图的检索匹配度实现快速筛查;结合保留时间、同位素丰度和多级特征碎片离子对目标化合物进行确证。该方法具有简便快速、准确、灵敏度高等优点,同时可实现无标准物质的情况下,较短时间内完成对食品中可能存在的添加剂和非法添物进行筛查检测,缩短检测时间,提高检测效率。

    Abstract:

    A method was developed screening, confirming and quantifying multiple additives and banned dyes in wine, juice and other beverages by liquid chromatography-ion trap-time of flight tandem mass spectrometry (LC-MS-IT-TOF). The accurate and multiple-stage mass spectrometry database of 41compounds was established. The analytes in samples were diluted with water-methanol (v/v). In the chromatographic analysis, target compounds were separated on a C18 column (150 mm × 4.6 mm, 5 μm) with the gradient elution using the mobile phases of methanol and 2 mM ammonium acetate. The results showed that the limits of detection were 0.005~1.0 mg/kg. The method validation was carried out at three spiking levels, and the recoveries were 41.2%~114.1%, with the relative standard deviations (RSDs) of 4.3%~16.4%. The screening of analytes was performed by precision mass matching and library searching. The retention time, isotopic abundance and multiple-stage ion mass spectral was employed in this confirmation. This method is simple, fast, credible and highly sensitive and can be applied to screening both multiple and illegal additives in foods without reference standards, reducing the analytical time and improving detection efficiency.

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张帆,颜鸿飞,戴洁云,等.食品多组分添加剂及非法添加物的HPLC—HRMS广谱筛查[J].食品与机械,2016,32(8):42-48,62.
ZHANGFan, YANHongfei, DAIJieyun, et al. Wide-scope screening of multiple and illegal additives in foods by high performance liquid chromatography-high resolution mass spectrometry[J]. Food & Machinery,2016,32(8):42-48,62.

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