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城市污水处理厂污泥中卤代甲基磺酸的液相色谱-串联质谱分析方法研究
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刘凯,史亚利,蔡亚岐,何绪文 1.中国矿业大学(北京)化学与环境工程学院2.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 
基金项目:国家水体污染控制与治理科技重大专项资助(2014ZX07405001)
中文摘要:建立了测定城市污水处理厂污泥样品中5种卤代甲基磺酸的高效液相色谱-串联质谱(HPLC-MS/MS)方法。通过对萃取溶剂、提取方式和萃取次数等条件进行优化,确定最佳萃取条件为:萃取溶剂为甲醇-水(体积比1∶1)混合溶液,摇床振荡提取1 h,萃取1次。在该条件下对一氯甲基磺酸(Cl-MSA)、二氯甲基磺酸(Cl2-MSA)、三氯甲基磺酸(Cl3-MSA)、一溴甲基磺酸(Br-MSA)和三氟甲基磺酸(F3-MSA)的萃取效率分别为(484±28)%、(683±09)%、(810±48)%、(380±11)%和(991±12)%。该方法的线性范围为005~50 μg·kg-1,相关系数(r)大于0991,各化合物的检出限(S/N=3)为0003~0018 μg·kg-1,定量下限为 0010~0059 μg·kg-1 ;对实际样品的加标回收率为738%~101%,相对标准偏差为23%~125%,可满足污泥样品中痕量卤代甲基磺酸的分析需求。
中文关键词:卤代甲基磺酸  污泥  高效液相色谱-串联质谱(HPLC-MS/MS)
 
Determination of Five Halogenated Methyl Sulfonic Acids in Sludge from Municipal Sewage Treatment Plant by HPLC-MS/MS
Abstract:A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was presented for the determination of five halogenated methyl sulfonic acids(HMSAs)in sludge from municipal sewage treatment plant.Through investigation on extract solvent,extraction method and times,the optimum conditions were obtained as follows:the mixture of methanol and water(1∶1,by volume)was selected as extraction solvent,samples were continually oscillated at 350 r/min for 1 hour,and extracted once.Under the optimized conditions,the extraction efficiencies were(484±28)%,(683±09)%,(810±48)%,(380±11)% and(991±12)% for chloromethanesulfonic acid,dichloromethanesulfonic acid,trichloromethanesulfonic acid,bromomethanesulfonic acid and trifluoromethanesulfonic acid,respectively.The calibration curves for the analytes were linear in the range of 005-50 μg·kg-1 with their correlation coefficients(r)larger than 0991.The limits of detection(LOD)of the method ranged from 0003 to 0018 μg·kg-1 for HMSAs,and the limits of quantitation(LOQ)were in the range of 0010-0059 μg·kg-1.The spiked recoveries for HMSAs in sewage sludge were in the range of 738%-101% with relative standard deviations of 23%-125%.
Key Words:halogenated methyl sulfonic acids  sewage sludge  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
引用本文:刘凯,史亚利,蔡亚岐,何绪文.城市污水处理厂污泥中卤代甲基磺酸的液相色谱-串联质谱分析方法研究[J].分析测试学报,2018,37(10):1274-1278.
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