超高效液相色谱串联质谱法测定残留丙烯酰胺

Determination Residual Acrylamide in Water Treatment Flocculant by UPLC-MS/MS

目的建立快速测定聚丙烯酰胺水处理剂中丙烯酰胺单体的方法。方法样品中加入同位素内标,经甲醇超声提取,0.2μm滤膜过滤后,选择ACQUITY UPLCHSS T3（1.8μm,2.1 mm×100 mm）为分析柱,甲醇和水为流动相,采用正离子扫描反应监测模式检测丙烯酰胺的含量。结果聚丙烯酰胺水处理剂中丙烯酰胺单体在0~1 000 ng/m L范围内线性关系良好,相关系数为1.0000,检出限为0.09μg/g,检测限为0.31μg/g,平均回收率〉98.5%,精密度RSD〈5.0%。结论该方法操作简单、灵敏度高,选择性好,准确度高,适用于聚丙烯酰胺水处理剂中丙烯酰胺单体的测定。

Objective To develop a method of quickly determining residual acrylamide in water treatment flocculant. Methods Samples were extracted by methanol and filtered through 0. 2 μm membrane filters,then the content of acrylamide was analyzed by UPLC-MS / MS using ACQUITY UPLCHSS T3（ 1. 8 μm,2. 1 mm × 100mm） column in a positive ion scan mode. The mobile phase was methanol and water. Acrylamide-d3 was used as an internal standard. Results The linear range was 0 ~ 1 000 ng / m L and the correlation coefficient was 1. 0000. The detection limit was 0. 09 μg / g. The average recoveries were more than 98. 5% and RSDs were less than 5%. Conclusions The method is simple,rapid,sensitive,accurate and applicable in the determination of residual acrylamide in water treatment flocculant.