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固相萃取-高效液相色谱-质谱联用法测痕量双酚A的方法优化
Optimization of Solid Phase Extraction-High Performance Liquid Chromatography-Mass Spectrometry for Determination of Trace Amounts of Bisphenol A
投稿时间:2019-06-25  修订日期:2020-12-24
DOI:10.19316/j.issn.1002-6002.2021.03.21
中文关键词:  双酚A  固相萃取  高效液相色谱-质谱联用  方法优化
英文关键词:bisphenol A  solid phase extraction  high performance liquid chromatography-mass spectrometry  method optimization
基金项目:四川省科技支撑计划"城市污水处理厂中环境激素类污染物双酚A处理技术研究"(2018SZ0299),"矿区环境风险控制与应急创新技术研究"(2019YFS0051)
作者单位
王恒 四川省环境政策研究与规划院, 四川 成都 610041 
刘骞 四川省环境政策研究与规划院, 四川 成都 610041 
张力 四川省生态环境科学研究院, 四川 成都 610041 
张东贺 成都信息工程大学, 四川 成都 610225 
吴怡* 四川省生态环境科学研究院, 四川 成都 610041 
通讯作者:吴怡*  四川省生态环境科学研究院, 四川 成都 610041  
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中文摘要:
      通过优化固相萃取和液相色谱条件,建立了固相萃取-高效液相色谱-质谱法测定水中双酚A的检测方法。水样经C18固相萃取柱净化并富集双酚A后,采用C18反相色谱柱XR-ODS(2.0 mm×100 mm,2.2 μm)分离,MRM负离子模式测定。结果表明:BPA浓度为5~200 ng/L范围内线性关系良好(相关系数为0.999 9),取样量500 mL,浓缩500倍时,方法检出限(LOD)和定量下限(LOQ)分别为2.0、8.0 ng/L。实际水样加标量为5、20 ng水平时,BPA的相对标准偏差(RSD,n=8)分别为8%和7%,回收率范围分别为82%~103%和90%~111%。
英文摘要:
      The method for the determination of bisphenol A in water by solid phase extraction-high performance liquid chromatography-mass spectrometry was established by optimizing the conditions of solid phase extraction and liquid chromatography. The content of bisphenol A in water sample was separated by C18 reverse phase column XR-ODS (2.0 mm×100 mm,2.2 μm) and determined by MRM negative ion mode after it was purified and enriched by C18 solid phase extraction column. The results showed the method had a good linear relationship (r=0.9999) in range of 5-200 ng/L,and when the sample was concentrated 500 times in volume of 500 mL,the method detection limit (LOD) and lower limit of quantitation (LOQ) were 2.0 ng/L and 8.0 ng/L,respectively. When the actual water sample was spiked at 5 ng and 20 ng,the relative standard deviations of BPA (RSD,n=8) were 8% and 7%, the recovery rates ranged from 82% to 103% and 90% to 111%, respectively.
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