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

Determination of Five Halogenated Methyl Sulfonic Acids in Sludge from Municipal Sewage Treatment Plant by HPLC-MS/MS

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(Cl_2-MSA)、三氯甲基磺酸(Cl_3-MSA)、一溴甲基磺酸(Br-MSA)和三氟甲基磺酸(F_3-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. 05~50μg·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. 018μg·kg^(-1),定量下限为0. 010~0. 059μg·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。

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 0.05-50μg·kg-1 with their correlation coefficients(r)larger than 0.991.The limits of detection(LOD)of the method ranged from 0.003 to 0.018μg·kg-1 for HMSAs,and the limits of quantitation(LOQ)were in the range of 0.010-0.059μg·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%.