饮用水中九种卤乙酰胺的高效液相色谱-三重四极杆质谱测定方法
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摘要
本文应用固相萃取前处理方法和高效液相色谱-三重四极杆电喷雾质谱(HPLC-ESI/tq MS),优化并建立了9种氯代和溴代乙酰胺的同时测定方法.结果显示,在流动相甲醇/水(5/95,V/V)、流速0.3 m L·min-1、正离子模式条件下,9种卤乙酰胺的线性范围是5—200μg·L~(-1)或10—500μg·L~(-1)(R2>0.99),9种卤乙酰胺检出限为0.5—9.2μg·L~(-1).经过比较HLB是最优的固相萃取柱.在0.02、0.2、0.5μg·L~(-1)的3个加标水平下,9种卤乙酰胺的回收率分别为61%—84%、60%—93%和70%—104%,相对标准偏差为1.7%—4.4%、1.1%—4.1%和0.8%—4.1%.
In this study,a new method for the simultaneous determination of nine chlorinated and brominated haloacetamides in drinking water was developed using solid phase extraction(SPE) and high performance liquid chromatography-triple quadropole mass spectrometry(HPLC-tq MS) with positive electron spray ionization. The optimized HPLC mobile phase was composed of methanol and water(5/95,V/V) with a flow rate of 0.3 m L·min-1. The linear ranges of the HPLC-tq MS method were 5—200 μg·L~(-1)or 10—500 μg·L~(-1)(R2> 0. 99) for the nine haloacetamides. The detection limits of the nine haloacetamides were 0.5—9.2 μg·L~(-1). HLB column was found to be the optimal SPE column. With the spiked concentrations of 0.02,0.2 and 0.5 μg·L~(-1),the recovery rates of the nine haloacetamides were 61%—84%, 60%—93% and 70%—104%, respectively(relative standard deviations were 1.7%—4.4%,1.1%—4.1% and 0.8%—4.1%,respectively).
In this study,a new method for the simultaneous determination of nine chlorinated and brominated haloacetamides in drinking water was developed using solid phase extraction(SPE) and high performance liquid chromatography-triple quadropole mass spectrometry(HPLC-tq MS) with positive electron spray ionization. The optimized HPLC mobile phase was composed of methanol and water(5/95,V/V) with a flow rate of 0.3 m L·min-1. The linear ranges of the HPLC-tq MS method were 5—200 μg·L~(-1)or 10—500 μg·L~(-1)(R2> 0. 99) for the nine haloacetamides. The detection limits of the nine haloacetamides were 0.5—9.2 μg·L~(-1). HLB column was found to be the optimal SPE column. With the spiked concentrations of 0.02,0.2 and 0.5 μg·L~(-1),the recovery rates of the nine haloacetamides were 61%—84%, 60%—93% and 70%—104%, respectively(relative standard deviations were 1.7%—4.4%,1.1%—4.1% and 0.8%—4.1%,respectively).
引文
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[11]CHU W H,GAO N Y,YIN D Q,et al.Trace detemination of 13 haloacetamides in drinking water using liquid chromatography triple quardrupole mass spectrometry with atmospheric pressure chemical ionization[J].Journal of Chromatography A,2012,1235:178-181.
[12]CHU W H,GAO N Y,YIN D Q,et al.Formation and speciation of nine haloacetamides,an emerging class of nitrogenous DBPs,during chlorination or chloramination[J].Journal of Hazardous Materials,2013,260:806-812.
[2]赵玉丽,李杏放.饮用水消毒副产物:化学特性与毒性[J].环境化学,2011,30(1):20-33.ZHAO Y L,LI X F.Disinfection by-products in drinking water:Chemical characteristics and toxicity[J].Environmental Chemistry,2011,30(1):20-33(in Chinese).
[3]TOM B,HUANG J,TEMPLETON M R,et al.Occurrence and control of nitrogenous disinfection by-product in drinking water:A review[J].Water Research,2011,45:4341-4354.
[4]CHU W H,GAO N Y,YANG D,et al.Formation of nitrogenous disinfection by-products from pre-chloramination[J].Chemosphere,2011,85(7):1187-1191.
[5]PRESSMAN J G,RICHARDSON S D,SPETH T F,et al.Concentration,chlorination,and chemical analysis of drinking water for disinfection byproduct mixture health effects research:U.S.EPA's four lab study[J].Environmental Science&Technology,2010,44(19):7184-7192.
[6]RICHARDSON S D,THRUSTON A D,KRASNER S W,et al.Integrated disinfection by-products mixtures research:Comprehensive characterization of water concentrates prepared from chlorinated and ozonated/postchlorinated drinking water[J].Journal of Toxicology and Environmental Health,2008,71(17):1165-1186.
[7]RICHARDSON S D,DEMARINI D M,KOGEVINAS M,et al.What's in the pool?A comprehensive identification of disinfection byproducts and assessment of mutagenicity of chlorinated and brominated swwimming pool water[J].Environmental Health Perspectives,2010,118:1523-1530.
[8]KRASNER S W,WEINBERG H S,RICHARDSON S D,et al.Occurrence of a new generation of disinfection byproducts[J].Environmental Science&Technology,2006,40(23):7175-7185.
[9]PLEWA M J,MUELLNER M G,RICHARDSON S D,et al.Occurrence,synthesis,and mammalian cell cytotoxicity and genotoxicity of haloacetamides:An emerging class of nitrogenous drinking water disinfection byproducts[J].Environmental Science&Technology,2008,42(3):955-961.
[10]楚文海,高乃云.气相色谱-质谱法检测饮用水新生含氮消毒副产物氯代乙胺[J].分析化学研究简报,2009,37(1):103-106.CHU W H,GAO N Y.Determination of emerging nitrogenous disinfection byproducts chlorinated haloacetamides using gas chromatography mass spectrometry[J].Chinese Journal of Analytical Chemistry,2009,37(1):103-106(in Chinese).
[11]CHU W H,GAO N Y,YIN D Q,et al.Trace detemination of 13 haloacetamides in drinking water using liquid chromatography triple quardrupole mass spectrometry with atmospheric pressure chemical ionization[J].Journal of Chromatography A,2012,1235:178-181.
[12]CHU W H,GAO N Y,YIN D Q,et al.Formation and speciation of nine haloacetamides,an emerging class of nitrogenous DBPs,during chlorination or chloramination[J].Journal of Hazardous Materials,2013,260:806-812.