知识与财富的链接
建立了直接进样同时测定水体中41种初级芳香胺化合物的超高效液相色谱-串联质谱方法(UPLC-MS/MS)。样品不净化,直接过0.22μm滤膜上机检测。采用Phenomenex Kinetex F5液相色谱柱(3 mm×100 mm,2.6μm)进行分离,以0.05%甲酸水溶液-甲醇作为流动相进行梯度洗脱,流速为0.45 mL?min-1。采用正离子模式电喷雾电离(ESI+),多反应监测(MRM)模式检测,标准曲线外标法定量。结果表明,41种初级芳香胺化合物在0.08～50μg·L~(-1)浓度范围内线性良好,相关系数为0.989 9～0.999 8,检出限(LOD)和定量限(LOQ)分别为0.01～0.15μg·L~(-1)和0.04～0.30μg·L~(-1)。3个不同浓度水平下,相对标准偏差(RSD)为2.31%～7.90%,5μg·L~(-1)浓度加标水平下,回收率在64.2%～110.3%,其中39种化合物的回收率80%。该方法简便快捷、目标物覆盖范围广、准确度和灵敏度高,适用于水体样品中初级芳香胺化合物的测定。
A ultra high-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was developed for the simultaneous determination of 41 primary aromatic amines(PAAs)in water. The samples were not purified, and were filtered through a 0.22 μm microporous membrane. The target compounds were separated on a Phenomenex Kinetex F5(3 mm×100 mm; 2.6 μm)column by gradient elution using 0.05% formic acid-methanol as the mobile phase at a flow rate of 0.45 mL·min-1. The MS/MS analysis was performed with an electrospray ion source in positive mode under multiple reaction monitoring mode, and the calibration curve was used for quantification. The results showed that there were good linear relationships for the 41 PAAs in the concentration range of 0.08~50.00 μg·L-1, and their correlation coefficients(r2)were between 0.989 9~0.999 8. The limits of detection and limits of quantitation were in the ranges of 0.01~0.15 μg·L-1 and 0.04~0.30 μg·L-1, respectively. The relative standard deviations for the 41 prohibited compounds at three spiked levels were in the range of 2.31%~7.90%. At the 5 μg·L-1 level, the recoveries of 39 compounds among the 41 PAAs were above 80%. With simple pretreatment, a wide target range, high accuracy, and high sensitivity, the method is suitable for the analysis of PAAs in water.
