ZHANGChen,YUJiao-jiao,LIULei,et al.Optimization of Online Solid-phase Extraction/Ultra Performance Liquid Chromatography/Mass Spectrometry for Determination of Acrylamide in Drinking Water Using Response Surface Methodology[J].China Water & Wastewater,2023,39(16):147-154.
响应面法优化在线SPE/UPLC/MS测定水中丙烯酰胺
- Title:
- Optimization of Online Solid-phase Extraction/Ultra Performance Liquid Chromatography/Mass Spectrometry for Determination of Acrylamide in Drinking Water Using Response Surface Methodology
- Keywords:
- drinking water; acrylamide; response surface; online solid?phase extraction; mass spectrometry
- 摘要:
- 基于响应面法优化在线固相萃取/超高效液相色谱/质谱法检测饮用水中丙烯酰胺的新方法，通过萃取优化、质谱条件优化确定最佳检测条件，并进行了方法技术指标评价。结果表明，当固相萃取柱为HLB柱、富集流动相为0.5%氨水溶液、洗脱液为0.1%甲酸溶液和95%甲醇溶液时，萃取回收率最高，达到80.2%。单因素实验和响应面曲线拟合表明：当离子源毛细管电压为0.57 kV、离子源温度为110.17 ℃、锥孔电压为29.10 kV、脱溶剂气温度为613.42 ℃时，仪器灵敏度达到4.83E6。基于最优条件下得出的方法检出限为0.002 9 μg/L，检测限为0.012 μg/L，方法平均回收率为100.38%，相对标准偏差为0.19%，相较于国标方法，具有预处理时间短、测定精密度高等优点。
- Abstract:
- This paper developed a new method for the detection of acrylamide in drinking water based on online solid?phase extraction-ultra performance liquid chromatography-mass spectrometry optimized by response surface methodology. The optimal detection conditions were determined by extraction optimization and mass spectrometry optimization, and the technical indicators of the method were evaluated. When the solid-phase extraction column was HLB column, the enrichment mobile phase was 0.5% ammonia solution and the eluent was 0.1% formic acid solution and 95% methanol solution, the extraction recovery rate reached the highest of 80.2%. The single factor experiment and response surface curve fitting showed that the sensitivity of the instrument reached 4.83E6 when the ion source capillary voltage was 0.57 kV, the ion source temperature was 110.17 ℃, the cone hole voltage was 29.10 kV and the desolvation gas temperature was 613.42 ℃. Based on the optimal conditions, the detection limit was 0.002 9 μg/L, the limit of detection was 0.012 μg/L, the average recovery rate was 100.38%, and the relative standard deviation was 0.19%. Compared with the national standard method, this method has the advantages of short pretreatment time and high precision.
相似文献/References:
[1]张晓,高圣华,金敏,等.饮用水中病毒的富集和检测技术概述[J].中国给水排水,2020,36(8):50.
[2]陈诗琦,刘成,沈海军,等.水厂失效生物活性炭的更换策略探讨[J].中国给水排水,2020,36(17):49.
CHEN Shi-qi,LIU Cheng,SHEN Hai-jun,et al.Discussion on Replacement Strategy of Invalidated Biological Activated Carbon in Drinking Water Plants[J].China Water & Wastewater,2020,36(16):49.
[3]郭庆园,王春苗,于建伟,等.饮用水中典型嗅味问题及其研究进展[J].中国给水排水,2020,36(22):82.
GUO Qing-yuan,WANG Chun-miao,YU Jian-wei,et al.Research Progress on Typical Taste and Odor Problems in Drinking Water[J].China Water & Wastewater,2020,36(16):82.
[4]严心涛,吴云良,查巧珍,等.流式细胞术在饮用水微生物检测中的应用及挑战[J].中国给水排水,2020,36(22):89.
YAN Xin-tao,WU Yun-liang,ZHA Qiao-zhen,et al.Applications and Challenges of Microbial Detection in Drinking Water by Flow Cytometry[J].China Water & Wastewater,2020,36(16):89.
[5]周子翀,杨旭,肖融,等.应对高藻原水的水厂多点加氯技术原理与应用[J].中国给水排水,2021,37(12):109.
ZHOU Zi-chong,YANG Xu,XIAO Rong,et al.Technical Principle and Application of Multi-point Chlorination in High Algae Water Treatment[J].China Water & Wastewater,2021,37(16):109.
[6]高雪,杨唯艺,雷培树.饮用水紫外线组合消毒技术发展现状[J].中国给水排水,2021,37(18):52.
GAO Xue,YANG Wei-yi,LEI Pei-shu.Development Status of the Combined Ultraviolet Disinfection Technology in Drinking Water[J].China Water & Wastewater,2021,37(16):52.
[7]杨晶博,王蔚蔚,刘丹,等.上海市饮用水安全保障技术标准体系研究[J].中国给水排水,2021,37(22):118.
YANG Jing-bo,WANG Wei-wei,LIU Dan,et al.Research on Technical Standard System of Drinking Water Security in Shanghai[J].China Water & Wastewater,2021,37(16):118.
[8]刘云帆,黎艳,崔迪,等.中美饮用水安全保障技术团体标准对比研究[J].中国给水排水,2021,37(22):133.
LIU Yun-fan,LI Yan,CUI Di,et al.Comparative Study of Group Standards for Drinking Water Security Technology between China and the United States[J].China Water & Wastewater,2021,37(16):133.
[9]寸黎辉,李碧莹,尹玉忠,等.石墨炉原子吸收光谱法监测水体中铊分析条件优化[J].中国给水排水,2021,37(24):124.
CUN Li-hui,LI Bi-ying,YIN Yu-zhong,et al.Optimization of Analysis Condition for Monitoring Thallium in Water by Graphite Furnace Atomic Absorption Spectrometry[J].China Water & Wastewater,2021,37(16):124.
[10]赵珍仪,高峰,郑军朝.基于可直饮目标的城市二次供水改造经验探讨[J].中国给水排水,2022,38(1):129.
ZHAO Zhen-yi,GAO Feng,ZHENG Jun-zhao.Discussion on Urban Secondary Water Supply Reconstruction Experience Based on the Goal of Fine Drinking Water[J].China Water & Wastewater,2022,38(16):129.