液相色谱三重四极杆质谱内标法测定水中丙烯酰胺

Determination of acrylamide in water by Triple Quadrupole LC-MS internal standard method

采用液相色谱三重四极杆质谱法测定水中丙烯酰胺。样品经过0.22μm PTFE针式过滤头过滤后直接进样,采用喷雾正离子ESI+和多重反应监测模式(MRM),内标法定量分析。加入同位素内标法用来抵消质谱离子化时的基质效应,及消除样品过滤处理过程中的差异影响。结果表明,丙烯酰胺浓度为0.10~10.0μg/L时,标准曲线线性良好,相关系数0.9990~0.9993,方法检出限为0.06μg/L,测定下限为0.24μg/L。对3种不同浓度的标准样品进行测定,相对标准偏差1.8%~4.0%,实际样品的加标回收率为90.7%~106%。该方法灵敏度高,重现性好,可用于地表水、饮用水中丙烯酰胺的测定。

Acrylamide in water was determined by Triple Quadrupole LC-MS method.Samples were directly injected after being filtered through a 0.22μm PTFE syringe filter,and quantitatively analyzed by applying spray positive ion ESI+and multiple response monitoring(MRM)under an internal standard method.Isotope interior label method was added to offset matrix effect during mass spectrometry ionization and eliminate the differences impact caused by the sample filtration process.The results showed that when the concentration of acrylamide ranged from 0.10µg/L to 10.0µg/L,the standard curve had good linearity with the correlation coefficient ranging from 0.9990 to 0.9993;the detection limit was 0.06µg/L,and the determination lower limit was 0.24µg/L.Three standard samples with different concentrations were measured,and the relative standard deviation was between 1.8%and 4.0%,while the actual sample recovery rate was between 90.7%and 106%.This method has high sensitivity and good reproducibility,and can be used for the determination of acrylamide in surface water and drinking water.