色谱

色谱 ›› 2017, Vol. 35 ›› Issue (4): 398-404.DOI: 10.3724/SP.J.1123.2016.10042

• 研究论文 • 上一篇    下一篇

固相萃取/液相色谱-串联质谱法测定食品中二甲基黄

李优1, 徐敦明2, 伊雄海1, 盛永刚1, 时逸吟1, 赵善贞1, 邓晓军1   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 厦门出入境检验检疫局, 福建 厦门 361026
  • 收稿日期:2016-10-19 出版日期:2017-04-08 发布日期:2013-07-30
  • 通讯作者: 伊雄海,Tel:(021)38620517,E-mail:yixh@shciq.gov.cn.
  • 基金资助:

    国家重大科学仪器设备开发专项（2013YQ15055705）；上海市技术性贸易措施应对专项（14TBT006，15TBT004，15TBT005）；上海市科委技术标准专项（15DZ0503201）；长三角科技合作项目（15395810100）.

Determination of dimethyl yellow in foods by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction

LI You1, XU Dunming2, YI Xionghai1, SHENG Yonggang1, SHI Yiyin1, ZHAO Shanzhen1, DENG Xiaojun1   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2016-10-19 Online:2017-04-08 Published:2013-07-30
  • Supported by:

    National Key Scientific Instrument Development Project (No. 2013YQ15055705); Shanghai Technical Barrier Trade Item (Nos. 14TBT006, 15TBT004, 15TBT005); Technical Standard Item of Shanghai Science and Technology Commission (No. 15DZ0503201); Yangtze River Delta Science and Technology Cooperation Project (No. 15395810100).

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摘要：

建立了液相色谱-串联质谱（LC-MS/MS）测定食品中二甲基黄（DMY）的分析方法。样品经乙酸乙酯提取，二甲基黄专用固相萃取小柱（ProElut DMY SPE）净化，XDB-C18色谱柱（50 mm×4.6 mm，1.8 μm）分离，并以5 mmol/L乙酸铵水溶液（含0.1%（v/v）甲酸）-乙腈（含0.1%（v/v）甲酸）为流动相，梯度洗脱，电喷雾正离子模式（ESI+）电离，多反应监测模式（MRM）检测，内标法定量。结果表明，DMY在0~50 μg/L范围内线性关系良好，相关系数（r2）均大于0.999。方法的检出限（LOD，S/N>3）和定量限（LOQ，S/N>10）分别为2 μg/kg和10 μg/kg。不同食品基质中，DMY在10、20和100 μg/kg的添加水平下的平均加标回收率为93.3%~98.9%，相对标准偏差为1.6%~3.9%（n=6）。该方法有效补偿了液相色谱-串联质谱检测过程中的离子化抑制效应，灵敏度和准确度高，适用于腐乳、辣椒酱、禽蛋、豆干、糖果和火腿中DMY的测定。

关键词: 二甲基黄, 固相萃取, 基质效应, 内标法, 食品, 液相色谱-串联质谱

Abstract:

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the determination of dimethyl yellow (DMY) in foods. The samples spiked with D5-dimethyl yellow (D5-DMY) as the internal standard were extracted with ethyl acetate, cleaned up by a ProElut DMY SPE column. The separation was performed on an XDB-C18 column (50 mm×4.6 mm, 1.8 μm) with the mobile phases of 5 mmol/L ammonium acetate aqueous solution containing 0.1% (v/v) formic acid and acetonitrile containing 0.1% (v/v) formic acid. The identification and quantitation of DMY was performed by MS/MS in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The quantitative analysis was carried out by internal standard method. A good linear relationship, with the correlation coefficient (r2) greater than 0.999, was found in the mass concentration range of 0-50 μg/L. The limit of detection (LOD, S/N>3) and the limit of quantitation (LOQ, S/N>10) were 2 μg/kg and 10 μg/kg, respectively. The recoveries of DMY in foods spiked with 10, 20 and 100 μg/kg varied from 93.3% to 98.9%, and the relative standard deviations (RSDs) were between 1.6% and 3.9% (n=6). The method can effectively correct the ionization suppression, and it is sensitive, accurate and suitable for the monitoring of DMY in sufu, chili sauce, egg, dried bean curd, candy and ham.

Key words: dimethyl yellow (DMY), foods, internal standard method, liquid chromatography-tandem mass spectrometry (LC-MS/MS), matrix effect (ME), solid phase extraction (SPE)

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