首页|饮用水中9种卤代苯醌的悬浮固化分散液液微萃取-液相色谱-质谱联用快速测定法

饮用水中9种卤代苯醌的悬浮固化分散液液微萃取-液相色谱-质谱联用快速测定法

扫码查看
目的 建立饮用水中9种卤代苯醌的悬浮固化分散液液微萃取-液相色谱-质谱联用分析方法.方法 向10 ml水样中加入1.5 g的NaCl,在0.3 ml甲醇作为分散剂的情况下,用20 μl的1-十二醇进行分散液液微萃取,离心后萃取剂在-20℃冰箱中凝固,沥干水分后加入80 μl甲醇复溶.以甲醇-0.2%甲酸水为流动相,经AcclaimTM RSLC120C18色谱柱(2.1 mm×100mm,2.2 μm)分离后,采用四极杆串联质谱仪电喷雾负离子模式和多反应监测(MRM)模式进行检测,外标法定量.结果 9种氯代苯醌化合物在50~2 000 ng/L的浓度范围内,所得回归方程的线性关系良好,RSD>0.99.该方法的检出限为4~20 ng/L;加标回收率为79.6%~121.3%,RSD为4.4%~14.7%.结论 该方法简单、快速,可用于饮用水中9种氯代苯醌的同时检测.
Rapid determination of halogenated benzoquinones in drinking water by suspension solidification dispersion liquid-liquid microextraction and liquid chromatography-mass mpectrometry
Objective To develop a suspension solidification dispersion liquid microextraction by liquid chromatography-mass spectrometry method for 9 types of chlorobenzoquinones in drinking water.Methods After 10 ml water was added into 1.5 g NaCl,the dispersed liquid-liquid microextraction was carried out by 20 μl 1-dodecanol which 0.3 ml methanol was the dispersant.After centrifugation,the extractant was solidified in a refrigerator at-20 ℃.Then re-solubilized was operated by adding 80 μl methanol when draining the water.The nine halogenated quinones were analyzed with the mobile phases of methanol and 0.2%formic acid in water,and then separated on an Acclaim TM RSLC120 C18 column(2.1 mmx100 mm,2.2μm).The detection was performed in electrospray negative ionization mode and multiple reaction monitoring(MRM)mode by quadrupole tandem mass spectrometer,and quantificated by tht external standard method.Results Nine chlorobenzoquinone compounds exhibited good linearity in the concentration range of 50-2 000 ng/L,with correlation coefficients not less than 0.99.The recoveries of the nine chlorobenzoquinone compounds spiked at three spiked levels were in the range of 79.6%-121.3%with the relative standard deviations(RSDs)of 4.4%-14.7%;the limits of detection were 4-20 ng/L.Conclusion The method is simple and fast,and it can be used for the simultaneous detection of 9 chlorobenzoquinones in drinking water.

Solidification floating organic droplet dispersion liquid microextractionHalogenated benzoquinoneLiquid mass spectrometryDrinking water

周华、黄琴、占炳东、吴香伦

展开 >

衢州市疾病预防控制中心理化检验科,浙江 324000

凝固漂浮有机液滴-分散液液微萃取 卤代苯醌 液质联用 饮用水

浙江省医药卫生科技计划项目衢州市科技计划竞争性项目

2023KY12972022K78

2024

环境与健康杂志
中华预防医学会,天津市疾病预防控制中心

环境与健康杂志

CSTPCD
影响因子:0.658
ISSN:1001-5914
年,卷(期):2024.41(1)
  • 13