色谱 ›› 2017, Vol. 35 ›› Issue (12): 1294-1300.DOI: 10.3724/SP.J.1123.2017.08014

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆静电场轨道阱高分辨质谱测定聚丙烯酰胺中丙烯酰胺单体的残留

王成龙1, 赵金利1, 李燕莹1, 梁兰兰2, 戚平1   

  1. 1. 广州市食品检验所, 广东 广州 510410;
    2. 广州城市职业学院, 广东 广州 510405
  • 收稿日期:2017-08-25 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 戚平,E-mail:gzsp2000@163.com
  • 基金资助:

    广东省自然科学基金项目(2016A030313564).

Determination and identification of acrylamide residues in poly-acrylamide by ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry

WANG Chenglong1, ZHAO Jinli1, LI Yanying1, LIANG Lanlan2, QI Ping1   

  1. 1. Guangzhou Institute for Food Control, Guangzhou 510410, China;
    2. Guangzhou City Polytechnic, Guangzhou 510405, China
  • Received:2017-08-25 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Natural Science Foundation of Guangdong Province (No. 2016A030313564).

摘要:

通过Hypercarb色谱柱分离,建立了四极杆静电场轨道阱高分辨质谱平行反应监测(PRM)模式检测聚丙烯酰胺(PAM)中单体残留量的方法。PAM经水稀释,高速搅拌溶解均匀,过0.22 μm水相滤膜后,直接用高分辨质谱Q Exactive采集数据。以Hypercarb色谱柱为分析柱,水和甲醇为流动相,柱温为20℃,采用PRM模式,提取目标化合物及其二级子离子的精确质量数,并对二级特征碎片进行同位素匹配,推测碎裂规律,以强化定性效果。结果表明:在2~50 μg/L范围内线性关系良好(相关系数为0.9998),方法检出限(LOD)可达到1.5 μg/kg,满足食品级PAM的检测要求。通过加标验证,回收率为101.3%~107.1%,相对标准偏差为3.1%~4.1%。实际样品验证结果表明,PAM中丙烯酰胺(AM)单体的残留质量分数范围为0~0.43%,存在一定的安全风险。该方法简单、准确、高效,可作为快检和确证检测技术广泛使用。

关键词: 丙烯酰胺, 超高效液相色谱, 聚丙烯酰胺, 四极杆静电场轨道阱高分辨质谱

Abstract:

A new method for the direct determination of acrylamide residues in poly-acrylamide (PAM) by ultra-performance liquid chromatography (UPLC)-quadrupole electrostatic field orbitrap high-resolution mass spectrometry with the Hypercarb column was developed. With being diluted by water, the PAM sample was dissolved well by high-speed stirring. After filtering through a 0.22 μm aqueous phase microporous membrane, the sample was analyzed by high-resolution mass spectrometry directly. Chromatographic analysis was carried out using a Hypercarb column, distilled water and methanol applied as the mobile phases. In addition, the column temperature was strictly set at 20℃. The sample was determined in the mode of parallel reaction monitoring (PRM). Accurate mass-to-charge ratio extraction of the target compound ion and its fragment ion were utilized with elemental composition analysis and isotope distribution of the fragment ion to further improve the accuracy of qualitative and quantitative analysis. Meanwhile, the fragmentation pattern of acrylamide was acquired. The calibration curve showed a good linearity in the range of 2-50 μg/L with the correlation coefficient of 0.9998. The limit of detection (LOD) was 1.5 μg/kg, satisfying the detection demands. The recoveries of the acrylamide were in the range of 101.3%-107.1%. The relative standard deviations (RSD) were 3.1%-4.1%. The applications indicated that the mass percentages of AM in PAM were in the range of 0-0.43%. The proposed method is easy, fast, sensitive and suitable for the determination and confirmation of acrylamide residues in PAM.

Key words: acrylamide (AM), poly-acrylamide (PAM), quadrupole electrostatic field orbitrap high-resolution mass spectrometry, ultra-performance liquid chromatography (UPLC)

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