固相萃取-超高效液相色谱-串联质谱法测定饮用水中12种卤代苯醌
Determination of twelve halobenzoquinones in drinking water by solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry
尹丹阳 1田丽 1王敏娟 1胡佳薇1
作者信息
- 1. 陕西省疾病预防控制中心,西安 710054
- 折叠
摘要
目的 建立固相萃取-超高效液相色谱-串联质谱同时测定饮用水中12种卤代苯醌的方法.方法 饮用水经甲酸酸化,Bond Elut Plexa固相萃取小柱净化和浓缩后,Waters ACQUITY HSS T3 柱(100mm×2.1 mm,1.8 μm)分离,以甲醇-0.1％甲酸水溶液梯度洗脱.质谱采用电喷雾负离子模式和多反应监测检测.采用空白基质匹配标准曲线法定量分析.结果 12种卤代苯醌至少在浓度为5.0～150.0 ng/mL的范围内呈良好线性关系,相关系数r＞0.999;方法 检出限低于2.0 ng/L,定量限低于5.0 ng/mL;加标回收率70.0％～84.0％,基质效应0.08～0.64.结论 本方法检测灵敏度高、准确性好、分析速度快,适用于饮用水中消毒副产物卤代苯醌类化合物的检测.
Abstract
OBJECTIVE To establish a method for twelve halobenzoquinones(HBQs)in drinking water by solid phase extraction-ultra-performance liquid chromatography coupled with electrospray-tandem mass spectrometry(SPE-UPLC-MS/MS).METHODS The drinking water was acidified with formic acid and concentrated by Bond Elut Plexa solid phase extraction column.The sample solution was separated using Waters ACQUITY HSS T3 column(100 mm × 2.1 mm,1.8 μm)with gradient elution using methanol-water containing 0.1％formic acid as mobile phase.The target compouds were detected in negtive electrospray ionization(ESI-)and multiple reaction monitoring.RESULTS The concentration of twelve HBQs showed good linearity in the range 5.0-150.0 ng/mL,respectively,with the correlation coefficients greater than 0.999.The limits of detection(LOD)of twelve HBQs were lower than 2.0 ng/mL,and the limits of quantification(LOQ)for twelve HBQs were lower than 5.0 ng/mL,respectively.The recoveries of three levels in the matrix were 70.0％-84.0％.The matrix effffect was 0.08-0.64.CONCLUSION The SPE-UPLC-MS/MS method has high sensitivity,good accuracy and fast analysis speed for the detection of halobenzoquinones in drinking water.
关键词
固相萃取-超高效液相色谱-串联质谱法/饮用水/消毒副产物/卤代苯醌Key words
solid phase extraction-ultra-performance liquid chromatography coupled with electrospray-tandem mass spectrometry/drinking water/disinfection byproducts/halobenzoquinones引用本文复制引用
出版年
2024
NETL
NSTL
万方数据