| 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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| 基金项目:国家水体污染控制与治理科技重大专项资助（2014ZX07405001） |
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| 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（484±28）%、（683±09）%、（810±48）%、（380±11）%和（991±12）%。该方法的线性范围为005~50 μg·kg-1，相关系数（r）大于0991，各化合物的检出限（S/N=3）为0003~0018 μg·kg-1，定量下限为 0010~0059 μg·kg-1 ；对实际样品的加标回收率为738%~101%，相对标准偏差为23%~125%，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） |
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| Determination of Five Halogenated Methyl Sulfonic Acids in Sludge from Municipal Sewage Treatment Plant by HPLC-MS/MS |
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| 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（484±28）%，（683±09）%，（810±48）%，（380±11）% and（991±12）% 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 005-50 μg·kg-1 with their correlation coefficients（r）larger than 0991.The limits of detection（LOD）of the method ranged from 0003 to 0018 μg·kg-1 for HMSAs，and the limits of quantitation（LOQ）were in the range of 0010-0059 μg·kg-1.The spiked recoveries for HMSAs in sewage sludge were in the range of 738%-101% with relative standard deviations of 23%-125%. |
| 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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