离子色谱-串联四极杆质谱对处理水中卤代乙酸的监测  

Monitor of Trace Disinfection By-Products Dichloroacetic Acid and Trichloroacetic Acid in Different-technique-treated Tap Waters by IC-ESI-MS/MS

作　　者：刘肖[1,2] 牟世芬[1] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室 [2]戴安中国有限公司应用研究中心,北京100085

出　　处：《净水技术》2007年第3期66-68,共3页Water Purification Technology

基　　金：国家重点基础研究计划(973项目)(NO.2003CB415001);国家自然科学基金(NO.20577058);中国科学院优秀博士论文科研基金资助项目

摘　　要：用离子色谱-串联电喷雾四极杆质谱联用技术测定不同饮用水消毒工艺产生卤代乙酸浓度的方法。该方法选用IonPac Prototype-10高容量阴离子交换柱为分离柱,以淋洗液自动发生装置在线产生不同浓度的KOH为淋洗液,实现对自来水样品中两种卤代乙酸和多种常见阴离子的完全分离,经抑制器将淋洗液抑制为近中性后,进入ESI-MS/MS质谱系统,选取适合的离子对和能量、温度等条件,进行准确定量分析。在优化的色谱和质谱条件下,二氯乙酸和三氯乙酸的检出限分别为0.053μg/L和0.46μg/L。峰面积校正曲线的线性范围均超过两个数量级,对四种不同浓度的标准溶液和实际样品连续9次进样,峰面积的相对标准偏差小于7%。挑选其中的典型样品进行不同浓度的标准加入实验,回收率在89.9%～108.0%之间。The present paper developed a new method on the determination of carcinogenic disinfection by-products （DBPs）-trace dichloroacetic acid and trichloroacetic acid in tap water samples by Ion Chromatography-Electrospray-Tandem Mass Spectrometry （IC-ESI-MS/MS）. The separation of two haloacetic acids （HAA2） and the other common inorganic anions in tap water was obtained by Dionex IonPac Prototype-10 high capacity column and KOH gradient eluents which were generated by Eluent Generator of ICS-3000 were selected. After the suppressor in which the eluents were suppressed to be neutral pH, API3200 ESI-MS/MS was employed to detect and measure analytes under appropriate MS conditions without adding any organic solvent. In the case of HAA2, optimised IC and MS parameters including eluent gradient, temperature and collision energy etc. brought high sensitivity in which the minimal detection limits （MDLs） of DCAA and TCAA were 0.053 μg/L and 0.46 μg/L while the linear coefficients （R） of calibration curves which might calibrate over two orders of magnitude were 0.9999 and 0.9992 respectively. RSDs were all lower than 7%.The recoveries of spiked standard were between 89.9%-108.0%.

关 键 词：二氯乙酸 三氯乙酸 离子色谱 串联质谱 臭氧 氯胺 

分 类 号：O623.64[理学—有机化学]