亲水色谱-质谱检测器联用测定水中三氟乙酸和二氯乙酸
|
摘要
目的建立快速、简单检测自来水中两种常见卤乙酸的亲水色谱-质谱定性定量分析方法。方法采用自来水样直接进样,经过氨基柱分离净化,应用90%10mmol/L乙酸铵-10%乙腈作为流动相进行等度洗脱,电喷雾负离子(ESI-)扫描模式,选择离子监测模式(SRM)进行质谱分析。结果目标化合物在3 min内实现分离,三氟乙酸(TFA)和二氯乙酸(DCAA)在检测质量浓度范围内均线性关系良好(r≥0.997),检测限为10～50μg/L,定量限为25～200μg/L,对三氟乙酸和二氯乙酸分别进行低、中、高3个浓度梯度的样品加标回收试验(n=3),平均加标回收率为74.3%～116%,相对标准偏差为1.3%～5.5%。结论该分析方法操作简单、精密度好、灵敏度高,适用于快速检测自来水中常见卤乙酸。
Objective To establish a rapid and simple qualitative and quantitative analysis method for 2 kinds of haloacetic acids(HAAs)in tap water by hydrophilic interaction chromatography tandem mass spectrometry(HILIC-MS).Methods Tap water samples were loaded directly into amino columns for separation and purification by applying 10% acetonitrile-90% 10 mmol/L ammonium acetate as mobile phase under isocratic elution mode.Electrospray ionization in the negative scanning model was applied with selected reaction monitoring(SRM)mode.Results Complete separation of target compounds were achieved in 3 min,trifluoroacetic acid(TFA)and dichloroacetic acid(DCAA)had good linearship in the detection range(r≥0.997).The limits of detection(LODs)were in the range of 10-50μg/L,while the limits of quantification(LOQs)were in the range of 25-200μg/L.The average recovery rates of HAAs at low,medium,high spiked concentration levels(n=3)were in the range of 74.3%-116%,the relative standard deviations(n=3)were in the range of 1.3%-5.5%.Conclusion The established method is suitable for rapid detection of common haloacetie acids in tap water for its convenience,good precision and high sensitivity.
Objective To establish a rapid and simple qualitative and quantitative analysis method for 2 kinds of haloacetic acids(HAAs)in tap water by hydrophilic interaction chromatography tandem mass spectrometry(HILIC-MS).Methods Tap water samples were loaded directly into amino columns for separation and purification by applying 10% acetonitrile-90% 10 mmol/L ammonium acetate as mobile phase under isocratic elution mode.Electrospray ionization in the negative scanning model was applied with selected reaction monitoring(SRM)mode.Results Complete separation of target compounds were achieved in 3 min,trifluoroacetic acid(TFA)and dichloroacetic acid(DCAA)had good linearship in the detection range(r≥0.997).The limits of detection(LODs)were in the range of 10-50μg/L,while the limits of quantification(LOQs)were in the range of 25-200μg/L.The average recovery rates of HAAs at low,medium,high spiked concentration levels(n=3)were in the range of 74.3%-116%,the relative standard deviations(n=3)were in the range of 1.3%-5.5%.Conclusion The established method is suitable for rapid detection of common haloacetie acids in tap water for its convenience,good precision and high sensitivity.
引文
[1]Ates N,Kaplan SS,Sahinkaya E,et al.Occurrence of disinfection by-products in low DOC surface waters in Turkey[J].J Hazard Mater,2007,142(1/2):526-534.
[2]雷颖,八十岛城,王凌云,等.液相色谱-串联质谱法同时检测自来水中9种卤乙酸[J].中国给水排水,2013,29(20):124-129.
[3]张晓健,李爽.消毒副产物总致癌风险的首要指标参数-卤乙酸[J].给水排水,2000,26(8):1-6.
[4]张颖,李金龙,张剑波.环境水体中三氟乙酸的存在现状及分析方法的研究[J].中国环境监测,2001,17(6):17-20.
[5]李祥平,齐剑英,陈永亨.离子色谱法测定环境水体中的卤乙酸和草甘膦[J].应用化学,2009,26(4):447-450.
[6]李少霞,梁旭霞,杨业,等.气相色谱法测定饮用水中的消毒副产物-卤乙酸[J].华南预防医学,2007,33(2):57-59.
[7]刘玉灿,段晋明,李伟.气相色谱-三重四级杆质谱联用法同时检测水中10种卤乙酸[J].分析化学,2014,42(1):77-82.
[2]雷颖,八十岛城,王凌云,等.液相色谱-串联质谱法同时检测自来水中9种卤乙酸[J].中国给水排水,2013,29(20):124-129.
[3]张晓健,李爽.消毒副产物总致癌风险的首要指标参数-卤乙酸[J].给水排水,2000,26(8):1-6.
[4]张颖,李金龙,张剑波.环境水体中三氟乙酸的存在现状及分析方法的研究[J].中国环境监测,2001,17(6):17-20.
[5]李祥平,齐剑英,陈永亨.离子色谱法测定环境水体中的卤乙酸和草甘膦[J].应用化学,2009,26(4):447-450.
[6]李少霞,梁旭霞,杨业,等.气相色谱法测定饮用水中的消毒副产物-卤乙酸[J].华南预防医学,2007,33(2):57-59.
[7]刘玉灿,段晋明,李伟.气相色谱-三重四级杆质谱联用法同时检测水中10种卤乙酸[J].分析化学,2014,42(1):77-82.