固相萃取-超高效液相色谱串联质谱法测定水中13种苯胺类化合物

Determination of 13 aniline compounds in water by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

建立了固相萃取-超高效液相色谱串联质谱法测定水中13种苯胺类化合物。样品通过HC-C18固相萃取小柱富集,洗脱后加入内标苯胺-D5进行氮吹浓缩,经HSS T3色谱柱(150 mm×2.1 mm,1.8μm)分离,采用多反应监测扫描模式,以内标法定量。13种苯胺类化合物在0.1~100μg/L(其中3-硝基苯胺为0.2~200μg/L)范围内与特征离子的色谱峰面积线性关系良好,相关系数均大于0.995,方法检出限为0.001~0.006μg/L,平均加标回收率为67.3%~117%,测定结果的相对标准偏差为3.77%~16.9%(n=6)。该法操作简单、稳定性好,能够满足实际水体中13种苯胺类化合物大批量样品分析的需求。

The determination of 13 aniline compounds in water by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry was developed.The samples were enriched by HC-C18 solid phase extraction cartridge.After elution,the internal standard aniline-D5 was added to concentrate by nitrogen blowing.The samples were separated by HSS T3 column(150 mm×2.1 mm,1.8μm),monitored in multiple reaction monitoring mode,and quantified by internal standard method.The 13 aniline compounds had good linear relationship with the chromatographic peak area of characteristic ions in the range of 0.1-100μg/L(among which 3-nitroaniline was 0.2-200μg/L),the correlation coefficients were all greater than 0.995,and the method detection limit was 0.001-0.006μg/L.The average spiked recoveries were 67.3%-117%,and the relative standard deviations of determination results were 3.77%-16.9%(n=6).The method is simple in operation and good in stability,and can meet the needs of large scale sample analysis of 13 aniline compounds in actual water.