色谱

色谱

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液相色谱/四极杆-飞行时间质谱法筛查奶酪中29种禁用和限用合成色素

赵延胜1,2, 杨敏莉1, 张峰1, 冯峰1, 储晓刚1*, 董英2   

  1. 1. 中国检验检疫科学研究院, 北京 100123; 2江苏大学, 江苏 镇江 212013
  • 收稿日期:2011-04-26 修回日期:2011-05-30 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 储晓刚,博士,研究员,研究方向为有害物质及其代谢机理
  • 基金资助:

    国家自然科学基金项目(91017013, 21005057, 31070327)

Stir rod sorptive extraction with poly(methacrylic acid-co-ethylene dimethacrylate) as coating and its application to the analysis of sulfonamides in milk samples

ZHAO Yansheng1,2, YANG Minli1, ZHANG Feng1, FENG Feng1, CHU Xiaogang1*, DONG Ying2   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 2. Jiangsu University, Zhenjiang 212013, China
  • Received:2011-04-26 Revised:2011-05-30 Online:2011-07-28 Published:2011-08-19

PDF

570

被引次数

79

摘要： 建立了奶酪样品中29种禁用和限用合成色素的液相色谱/四极杆-飞行时间质谱(LC/Q-TOF MS)筛查方法。样品经正己烷-水(3:1, v/v)振荡提取,得到正己烷层、水层和残渣3部分。正己烷层经旋转蒸发浓缩后,用乙酸乙酯-环己烷(1:1, v/v)溶解,经过凝胶渗透色谱(GPC)净化去除油脂。水层经乙腈振荡提取,得到乙腈-水提取液。残渣经氨水-甲醇(1:99, v/v)溶液振荡提取,得到氨水-甲醇提取液。乙腈-水提取液和氨水-甲醇提取液不需净化直接分析。结果表明: 29种不同极性范围的合成色素化合物分别得到了有效的提取,提取回收率为70%～95%。而Q-TOF MS提供的精确质量数定性功能可以将不同种类的合成色素化合物筛查出来,各化合物与精确质量质谱库中化合物的匹配度为59.66～99.47。通过Target MS/MS扫描方式进行定量,得到8种苏丹类化合物的方法检出限为0.4～2.5 μg/kg, 21种水溶性合成色素及染料化合物的检出限为20～80 μg/kg。该方法对禁用和限用合成色素的筛查范围广泛,对含有蛋白质、脂肪等基质的食品具有较好的适用性。

关键词: 合成色素, 奶酪, 筛查, 液相色谱/四极杆-飞行时间质谱

Abstract: A poly(methacrylic acid-co-ethylene dimethacrylate) polymer (poly(MAA-co-EDMA)) was prepared via in-situ polymerization on the outside surface of vial glass insert and used as stir rod sorptive extraction (SRSE) coating. The extraction performance of the polymer coating toward four sulfonamides (SAs) was investigated. The effects of several parameters to SRSE, such as the pH value, inorganic salt and organic phase concentrations of the sample matrix, were investigated. It demonstrated that the sulfonamides were captured on the poly(MAA-co-EDMA) coating mainly through cation-exchange and hydrophobic interactions. A novel approach is presented for the determination of four sulfonamide antibacterial residues in milk samples by coupling SRSE to liquid chromatography and electrospray ionization mass spectrometry (SRSE/LC-ESI-MS). In this method, the detection limits (S/N=3) of 0.11~0.52 μg/L and quantification limits (S/N=10) of 0.35~1.72 μg/L were obtained. The method showed good linearity in the range of 1~500 μg/L. Good method reproducibility was also found by intra- and inter-day precisions, yielding the relative standard deviations (RSDs) less than 11.3%. The results demonstrated that the proposed method is simple, sensitive, low cost and suitable for the determination of sulfonamides in milk samples.

Key words: milk, poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)), sulfonamides (SAs), stir rod sorptive extraction (SRSE)