摘要
建立固相萃取-超高效液相色谱-串联质谱(UHPLC-MS/MS)测定生活饮用水及聚丙烯酰胺化学处理剂中丙烯酰胺的方法。样品经椰子壳活性炭固相萃取小柱富集和净化,洗脱液经氮吹浓缩后用水复溶,采用UHPLC-MS/MS法测定,用同位素内标法定量。生活饮用水、聚丙烯酰胺化学处理剂中丙烯酰胺的质量浓度分别在0~50、10~500 ng/mL范围内与目标物与内标色谱峰面积的比值线性关系良好,相关系数分别为0.993和0.998。生活饮用水中丙烯酰胺的方法检出限为0.01μg/L,定量限为0.02μg/L,样品加标平均回收率为96.2%~99.9%,测定结果的相对标准偏差为2.6%~4.3%(n=6);聚丙烯酰胺化学处理剂中丙烯酰胺的方法检出限为0.005 mg/kg,定量限为0.01 mg/kg,样品加标平均回收为97.6%~100%,相对标准偏差为1.7%~5.5%(n=6)。该方法适用于生活饮用水及化学处理剂中丙烯酰胺的日常检测。
A method was established for the determination of acrylamide in drinking water and polyacrylamide chemical treatment agents by solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The samples were purified and enriched by coconut powdered activated carbon solid-phase extraction column,and the eluent was concentrated by nitrogen blowing and redissolved in water.UHPLC-MS/MS method was used for determination,and isotope internal standard method was used for quantification.The mass concentration of acrylamide in drinking water and polyacrylamide chemical treatment agents had good linear relationship with the ratios of chromatographic peak areas of the target compound to the internal standard in the range of 0-50 and 10-500 ng/mL,respectively,with correlation coefficients of 0.993 and 0.998,respectively.The detection limit of acrylamide in drinking water was 0.01μg/L,the quantification limit was 0.02μg/L,the average recoveries of samples spiked were 96.2%-99.9%,and the relative standard deviations of the determination results were 2.6%-4.3%(n=6).The detection limit of acrylamide in polyacrylamide chemical treatment agent was 0.005 mg/kg,the quantification limit was 0.01 mg/kg,the average recoveries of samples spiked were 97.6%-100%,and the relative standard deviations of the determination results for six parallel samples were 1.7%-5.5%.The developed method is suitable for routine determination of acrylamide in drinking water and chemical treatment agents.
作者
王鑫楠
凌映茹
王溪
刘运明
刘华良
WANG Xinnan;LING Yingru;WANG Xi;LIU Yunming;LIU Hualiang(Jiangsu Province Center for Disease Prevention and Control,Nanjing 210009,China)
出处
《化学分析计量》
2026年第1期80-86,共7页
Chemical Analysis And Meterage
基金
江苏省卫生健康委员会(BE2023772)
江苏省卫生健康委科研课题(Ym2023041)。
关键词
丙烯酰胺
生活饮用水
椰子壳活性炭
固相萃取
化学处理剂
超高效液相色谱-串联质谱法
acrylamide
drinking water
coconut powdered activated carbons
solid-phase extraction
chemical treatment agents
ultra high performance liquid chromatography-tandem mass spectrometry
