固相萃取-超高效液相色谱串接四级杆质谱同时测定调味品中12种工业染料
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赵榕 女 副主任技师 研究方向为食品中污染及营养成分 E-mail lxyue@yeah.net

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北京卫生局 北京市中医管理局青年科学研究资助项目(QN2007-16)


Simultaneous Determination of 12 Kinds of Industrial Dyes in Condiment by SPE-UPLC-MS/MS Method
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    摘要:

    目的 建立调味品中苏丹橙、苏丹黄、苏丹Ⅰ~Ⅳ、溶剂蓝35、对位红、苏丹黑B、苏丹红7B、苏丹红G、苏丹棕等工业染料的固相萃取-超高效液相色谱串接四级杆质谱(SPE-UPLC-MS/MS)测定方法。方法 以含10%乙醇的丙酮溶液作为提取溶剂,利用MAX强阴离子交换固相萃取柱(60 mg,3ml)对样品进行净化,UPLC-Ms/Ms测定试样中12种工业染料的含量。结果 方法的线性范围:对位红10.0~800.0 ng/ml ,其他11种染料5.0~400.0 ng/ml。12种工业染料的定性检出限为0.3~10.4μg/kg。定量检出限为0.8~31.2μg/kg。高、中、低3个浓度水平的加标回收率77.1%~141.9%,相对标准偏差5.5%~26.4%。结论 本方法灵敏、准确,可用于调味品中苏丹橙、苏丹黄、苏丹Ⅰ~Ⅳ、溶剂蓝35 、对位红、苏丹黑B、苏丹红7B、苏丹红G、苏丹棕等12种非法添加的工业染料的同时测定及确证。

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    Objective To established a method for simultaneous determination of Sudan Orange,Sudan Yellow,Sudan Ⅰ?Ⅳ,Solvent Blue 35,Para Red,Sudan Black B,Sudan Red 7B,Sudan Red G and Sudan Brown in condiment and meat by solid-phase extraction and ultra performance liquid chromatography electrospray ionization-tandem mass spectrometry(SPE-UPLC-MS/MS)method. Method The samples were extracted by acetone containing 10% ethanol and cleaned-up by OASIS MAX solid phase extraction column (60mg,3ml). The dyes were determined by UPLC-MS/MS. Results The linear range was 10.0-800.0 ng/ml for Para Red and 5.0-400.0ng/ml for the other 11 compounds, the correlation coefficients were >0.99. The qualitative detection limits of the method were in the range of 0.3-10.4μg/kg and the quantitative detection limits of the method were in the range of 0.8-31.2μg/kg. The average recoveries of adding standard at three levels were 77.1%?141.9% and the relative standard deviation (RSD) of the method was 5.5%?26.4%. Conclusion The method is sensitive, accurate and could be used for detecting 12 kinds of industrial dyes simultaneously in condiments.

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赵 榕,李 兵,赵海燕,薛 颖,吴国华,刘 伟,赵 耀.固相萃取-超高效液相色谱串接四级杆质谱同时测定调味品中12种工业染料[J].中国食品卫生杂志,2010,22(4):305-311.

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  • 收稿日期:2009-06-20
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