西北师范大学学报（自然科学版）2019，Vol.55Issue(1)：73-78,6.DOI:10.16783/j.cnki.nwnuz.2019.01.013
固相萃取联合液相色谱-三重四级杆质谱测定饮用水中的亚硝胺类物质
Determination of nitrosamine in drinking water by SPE and LC-TQMS
摘要
Abstract
Solid phase extraction (SPE) is performed by using coconut shell activated carbon small column for nitrosamines in water sample, SB-C8column is used as the separation column stationary phase, and the mixture of methanoic acid and methanol mixed in different ratios is used as mobile phase in gradient elution.Atmospheric pressure chemical ionization and multi-reactions monitor modes are used.A liquid chromatography-triple quadrupole mass spectrometry (LC-TQMS) method combined with solid-phase extraction (SPE) technique is developed for the determination of 8nitrosamine disinfection by-products in drinking water.The effects of loading time, elution volume, nitrogen blowing time and pH on recovery rate are investigated, and the solid-phase extraction process is optimized.The results show that the higher recovery rate can be achieved under the conditions of 1.5hof loading time, 13mL of elution volume, 60min of nitrogen blowing time and pH 8.0during the solid-phase extraction.The correlation coefficients of the standard calibration curves of the 8nitrosamines are greater than 0.99in the range of 1～100μg·L-1.The standard addition recovery rates are ranged from 67.05％to 91.37％with the relative standard deviations from 3.08％to 9.23％ (n=6) .Method detection limit (MDL) and instrument detection limit (IDL) are0.55～3.12μg·L-1 and 0.12～1.95μg·L-1, respectively.关键词
固相萃取/液相色谱-三重四级杆质谱/亚硝胺类消毒副产物/测定Key words
solid phase extraction (SPE)/liquid chromatography-triple quadrupole mass spectrometry (LC-TQMS)/nitrosamine disinfection by-products/determination分类
化学化工引用本文复制引用
范文哲,姜遥,黄正根,王光辉..固相萃取联合液相色谱-三重四级杆质谱测定饮用水中的亚硝胺类物质[J].西北师范大学学报（自然科学版）,2019,55(1):73-78,6.基金项目
国家自然科学基金资助项目(41761069) （41761069）
江西省自然科学基金资助项目(20181ACB20004) （20181ACB20004）
