摘要
建立了一种快速、灵敏分析自来水中9种卤乙酸的液相色谱一串联质谱(LC—MS/MS)同时定量检测方法。样品经O.45μm的膜过滤后,在Shim—pakXR—ODS色谱柱(3mm×75mm,2μm)上进行分离,采用甲醇-0.1%甲酸溶液梯度洗脱方式,电喷雾负离子(ESI-)模式,多反应监测模式(MRM)进行质谱分析。实验表明9种卤乙酸在检测范围内均具有良好的线性关系(帮〉0.9950),检测限(S/N〉3)为0.016~2.31μg/L,定量限(s/N〉10)为0.053~7.69μg/L;根据卤乙酸不同定量限分别进行低、中、高三个浓度梯度的空白加标实验(n=5),平均回收率为92.8%~107.2%,相对标准偏差为0.58%~12.8%;自来水基底加标实验(n=7)的平均回收率在83.9%~111.3%,相对标准偏差范围在1.6%~9.2%。该分析方法快速简便、灵敏度高、重现性好,可用于自来水中微量卤乙酸的快速检测。
A simple and rapid detection method for nine haloacetic acids (HAAs) in tap water was developed using liquid chromatography tandem mass spectrometry (LC-MS/MS). After being filtered through a 0.45 μm membrane, the samples were separated on a Shim-pak XR-ODS column (3 mm 75 mm, 2 μm) by applying methanol and Milli-Q water (containing 0.1% formic acid) as the mobile phase with gradient elution mode. Electrospray ionization was applied and operated in the negative multiple re- action monitoring (MRM) mode. The results showed that the linear correlation coefficients (R2) were larger than 0. 995 0, the limits of detection (S/N 〉 3) were in the range of 0. 016 to 2.31 ~xg/L, and the limits of quantification (LOQ) ( S/N 〉 10) were in the range of 0. 053 to 7.69 ~g/L. According to dif- ferent LOQ, the mean recoveries of HAAs spiked at three concentration levels (n = 5) in Milli-Q water were in the range of 92.8% to 107.2% , and the relative standard deviations (RSDs) were between 0.58% and 12.8%. Furthermore, the mean recoveries of HAAs spiked at 10 txg/L in tap water (n =7) were in the range of 83.9% to 111.3% , and the RSDs were between 1.6% and 9.2%. This method is suitable for rapid detection of trace haloacetic acids in tap water for its rapidity, convenience, high sensi- tivity and good reproducibility.
出处
《中国给水排水》
CAS
CSCD
北大核心
2013年第20期124-129,共6页
China Water & Wastewater
基金
国家水体污染控制与治理科技重大专项(2009ZX07423-001)
水利部公益性行业专项(201201033)
广东省科技计划项目(2012B030800001)
关键词
自来水
液相色谱-串联质谱
卤乙酸
tap water
liquid chromatography-tandem mass spectrometry
haloacetic acid