色谱2017，Vol.35Issue(12)：1294-1300,7.DOI:10.3724/SP.J.1123.2017.08014
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
Determination and identification of acrylamide residues in poly-acrylamide by ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry
摘要
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 filte-ring 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 paral-lel reaction monitoring( PRM ). Accurate mass-to-charge ratio extraction of the target com-pound 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.关键词
超高效液相色谱/四极杆静电场轨道阱高分辨质谱/丙烯酰胺/聚丙烯酰胺Key words
ultra-performance liquid chromatography( UPLC )/quadrupole electrostatic field orbitrap high-resolution mass spectrometry/acrylamide( AM)/poly-acrylamide( PAM)分类
化学化工引用本文复制引用
王成龙,赵金利,李燕莹,梁兰兰,戚平..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[J].色谱,2017,35(12):1294-1300,7.基金项目
广东省自然科学基金项目(2016A030313564).Natural Science Foundation of Guangdong Province( No. 2016A030313564). （2016A030313564）
