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.
作者
霍宗利
余囉
张婧婧
HUO Zong-li;YU Meng;ZHANG Jing-jing(Jiangsu Provincial Center for Disease Control and Prevention, Jiangsu Nanjing 210009, China)
出处
《江苏预防医学》
CAS
2019年第2期134-135,225,共3页
Jiangsu Journal of Preventive Medicine
基金
江苏省青年医学人才项目(QNRC2016543)