高效液相色谱串联质谱法测定聚丙烯酰胺残留单体

目的 建立聚丙烯酰胺水处理剂及饮用水中丙烯酰胺的高效液相色谱-串联质谱测定方法。方法 聚丙烯酰胺处理剂直接用甲醇超声提取,水样通过活性炭固相萃取柱富集,甲醇洗脱,采用T3色谱柱分离,以甲醇-0.1%甲酸水溶液作为流动相,以多反应监测(multiple reaction monitoring,MRM),ESI⁺电离方式,外标法定量。结果 丙烯酰胺在1.0～100.0 μg/L和0.50～10.0 mg/L质量浓度范围内线性良好,相关系数分别为0.999 3和0.999 8,方法回收率为95.0%～102%,RSD≤4.7%,方法检出限分别为2 μg/kg和0.000 2 μg/L。结论 该方法快速、准确、灵敏,适合聚丙烯酰胺水处理剂和饮用水中丙烯酰胺的测定。

Determination of residual monomer from polyacrylamide by high performance liquid chromatography-tandem mass spectrometry

Objective To develop an analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the determination of residual acrylamide in polyacrylamide water treatment agent and drinking water. Methods Polyacrylamide samples were extracted by ultrasonic with methanol, while water samples were concentrated through an active carbon cartridge. The chromatographic separation was performed on T3 column using a mobile phase consisting of methanol and 0.1% formic acid aqueous solution. The MS/MS detection was performed under the multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI⁺). Results The calibration curve of acrylamide showed a good linearity in the ranges of 1.0-100.0 μg/L (r=0.999,3) and 0.50-10.0 mg/L (r=0.999,8). The recoveries of acrylamide were in the range of 95.0%-102%. The relative standard deviation (RSD) was ≤ 4.7%, and the limits of detection were 2 μg/kg and 0.000,2 μg/L respectively. Conclusions The proposed method is fast, accurate, sensitive, and suitable for the quantification of residual acrylamide monomer in polyacrylamide water treatment agent and drinking water.