磁性聚苯乙烯-Fe3O4固相萃取-超高效液相色谱-串联质谱法测定水中双酚A
Determination of Bisphenol A in Water by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry after Solid Phase Extraction with Magnetic Polystyrene-Fe3O4
摘 要
建立了磁性聚苯乙烯-Fe3O4（HCP-Fe3O4）固相萃取联用超高效液相色谱-串联质谱（UHPLC-MS/MS）的检验方法，用于测定水中双酚A （BPA）的含量。水样经HCP-Fe3O4固相萃取，用甲醇洗脱后进样，以ACQUITY UPLC BEH C18色谱柱为分离柱，以不同体积比的甲醇和水作为流动相进行梯度洗脱；质谱分析采用电喷雾负离子（ESI-）模式电离、多反应监测（MRM）模式检测。BPA的质量浓度在1.000~1 000 μg·L-1内与其峰面积呈线性关系，方法的检出限（3S/N）为0.04 μg·L-1。加标回收率为98.4%~99.9%，测定值的相对标准偏差（n=6）为2.6%~8.2%。
固相萃取
超高效液相色谱-串联质谱法
双酚A
magnetic polystyrene-Fe3O4
solid phase extraction
ultra-high performance liquid chromatography-tandem mass spectrometry
bisphenol A
Abstract
A method of solid phase extraction with magnetic polystyrene-Fe3O4 (HCP-Fe3O4) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established, which was used to determine the content of bisphenol A (BPA) in water. After extracted by HCP-Fe3O4 and eluted by methanol, water samples were separated by ACQUITY UPLC BEH C18 column, with the mixtures of methanol and water with the different volume ratios as mobile phase for gradient elution. The electrospray ionization source of MS in negative ion (ESI-) mode was used for detection under the mode of multiple reaction monitoring (MRM). Linearity relationship between values of mass concentration of BPA and its peak area was kept in the range of 1.000-1 000 μg·L-1, with limit of detection (3S/N) of 0.04 μg·L-1. Values of the spiked recovery were found in the range of 98.4%-99.9%, and RSDs (n=6) of the measured values were found in the range of 2.6%-8.2%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202105013
所属栏目 专题报道(串联质谱法)
基金项目
收稿日期 2020/3/31
修改稿日期
网络出版日期
作者单位点击查看
备注秦园,中级检验师,硕士,主要从事水质、食品检验和液相色谱-串联质谱技术的应用研究工作
引用该论文: QIN Yuan,QIAN Zhirong,WU Mei,WU Jianbing,WANG Huifang,CHEN Zhujun. Determination of Bisphenol A in Water by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry after Solid Phase Extraction with Magnetic Polystyrene-Fe3O4[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(5): 459～462
秦园,钱志荣,吴梅,吴建兵,王惠芳,陈祝军. 磁性聚苯乙烯-Fe3O4固相萃取-超高效液相色谱-串联质谱法测定水中双酚A[J]. 理化检验－化学分册, 2021, 57(5): 459～462
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】潘胜东,何仟,陈晓红,等.固相萃取-超高效液相色谱-高分辨质谱法快速测定食用油中4种酚类环境雌激素残留[J].色谱, 2017,35(9):980-986.
【2】余建,宋紧东,蒋小良.环境水样中双酚A检测与分析方法的研究进展[J].日用化学品科学, 2014,37(4):32-36.
【3】牛宇敏,张晶,张书军,等.同位素稀释液相色谱-串联质谱法测定动物性食品中的双酚A、壬基酚及辛基酚[J].分析化学, 2012,40(4):534-538.
【4】XIAO J, SHAO B, WU X Y, et al. A study on bisphenol A, nonylphenol, and octylphenol in human urine samples detected by SPE-UPLC-MS[J]. Biomedical and Environmental Sciences, 2011,24(1):40-46.
【5】李延,胡双庆,尹大强,等.11种取代酚类内分泌干扰活性的初步筛选与评价[J].环境化学, 2003,22(4):385-389.
【6】郁蕾,尹燕敏,顾海东,等.超高效液相色谱-串联质谱法测定水中痕量双酚A[J].环境监测管理与技术, 2014,26(2):37-38.
【7】陈东洋,冯家力,张昊,等.固相萃取/高效液相色谱法测定饮用水中苯并(a)芘及双酚A[J].分析测试学报, 2015,34(7):848-851.
【8】邹荣婕,邓旭修,王斌,等.黄河调水调沙对黄河口海域双酚A的影响[J].生态学报, 2015,35(2):263-269.
【9】SHI J H, LIU X W, CHEN Q C, et al. Spatial and seasonal distributions of estrogens and bisphenol A in the Yangtze River Estuary and the adjacent East China Sea[J]. Chemosphere, 2014,111:336-343.
【10】王露,汪怡,杭学宇,等.磁性高交联聚苯乙烯-纳米Fe3O4的制备及其在牛奶中磺胺类药物检测中的应用[J].分析试验室, 2016,35(9):1052-1055.
【11】贺敏岚,李伟,苏鑫,等.纳米磁性材料在水处理领域的研究进展[J].化工新型材料, 2015,43(11):28-29.
【12】赵国平,莫尊理,王博,等.磁性Fe3O4纳米复合材料的研究进展[J].化工新型材料, 2015,43(6):10-13.
【13】WANG H Y, CAMPIGLIA A D. Direct determination of benzo[a]pyrene in water samples by a gold nanoparticle-based solid phase extraction method and laser-excited time-resolved Shpol'skii spectrometry[J]. Talanta, 2010,83(1):233-240.
【14】杨金泉,贺小敏,施敏芳,等.固相萃取-超高效液相色谱-串联质谱法测定饮用水中双酚A和双酚S[J].食品科学, 2019,40(20):332-337.
【15】刁春鹏,李聪,彭辉,等.基于磁性多壁碳纳米管的涡旋辅助分散基质固相萃取-高效液相色谱检测水中双酚A[J].中国环境监测, 2016,32(5):111-115.
【16】王利民,卢玉英,张磊,等.磁性活性炭分散固相萃取-液相微萃取-液相色谱检测水中痕量双酚A[J].广东化工, 2018,45(17):173-175.
【17】毛丽莎,刘桂华,姜杰,等.固相萃取-LC-MS/MS测定水中双酚A类物质[J].实用预防医学, 2016,23(10):1260-1263.
【18】郑赛,杨蕴嘉,张昕,等.超高效液相色谱-四极杆串联质谱法检测饮用水中双酚A和双酚F及其氯化消毒副产物[J].中国食品卫生杂志, 2017,29(2):155-159.
【2】余建,宋紧东,蒋小良.环境水样中双酚A检测与分析方法的研究进展[J].日用化学品科学, 2014,37(4):32-36.
【3】牛宇敏,张晶,张书军,等.同位素稀释液相色谱-串联质谱法测定动物性食品中的双酚A、壬基酚及辛基酚[J].分析化学, 2012,40(4):534-538.
【4】XIAO J, SHAO B, WU X Y, et al. A study on bisphenol A, nonylphenol, and octylphenol in human urine samples detected by SPE-UPLC-MS[J]. Biomedical and Environmental Sciences, 2011,24(1):40-46.
【5】李延,胡双庆,尹大强,等.11种取代酚类内分泌干扰活性的初步筛选与评价[J].环境化学, 2003,22(4):385-389.
【6】郁蕾,尹燕敏,顾海东,等.超高效液相色谱-串联质谱法测定水中痕量双酚A[J].环境监测管理与技术, 2014,26(2):37-38.
【7】陈东洋,冯家力,张昊,等.固相萃取/高效液相色谱法测定饮用水中苯并(a)芘及双酚A[J].分析测试学报, 2015,34(7):848-851.
【8】邹荣婕,邓旭修,王斌,等.黄河调水调沙对黄河口海域双酚A的影响[J].生态学报, 2015,35(2):263-269.
【9】SHI J H, LIU X W, CHEN Q C, et al. Spatial and seasonal distributions of estrogens and bisphenol A in the Yangtze River Estuary and the adjacent East China Sea[J]. Chemosphere, 2014,111:336-343.
【10】王露,汪怡,杭学宇,等.磁性高交联聚苯乙烯-纳米Fe3O4的制备及其在牛奶中磺胺类药物检测中的应用[J].分析试验室, 2016,35(9):1052-1055.
【11】贺敏岚,李伟,苏鑫,等.纳米磁性材料在水处理领域的研究进展[J].化工新型材料, 2015,43(11):28-29.
【12】赵国平,莫尊理,王博,等.磁性Fe3O4纳米复合材料的研究进展[J].化工新型材料, 2015,43(6):10-13.
【13】WANG H Y, CAMPIGLIA A D. Direct determination of benzo[a]pyrene in water samples by a gold nanoparticle-based solid phase extraction method and laser-excited time-resolved Shpol'skii spectrometry[J]. Talanta, 2010,83(1):233-240.
【14】杨金泉,贺小敏,施敏芳,等.固相萃取-超高效液相色谱-串联质谱法测定饮用水中双酚A和双酚S[J].食品科学, 2019,40(20):332-337.
【15】刁春鹏,李聪,彭辉,等.基于磁性多壁碳纳米管的涡旋辅助分散基质固相萃取-高效液相色谱检测水中双酚A[J].中国环境监测, 2016,32(5):111-115.
【16】王利民,卢玉英,张磊,等.磁性活性炭分散固相萃取-液相微萃取-液相色谱检测水中痕量双酚A[J].广东化工, 2018,45(17):173-175.
【17】毛丽莎,刘桂华,姜杰,等.固相萃取-LC-MS/MS测定水中双酚A类物质[J].实用预防医学, 2016,23(10):1260-1263.
【18】郑赛,杨蕴嘉,张昕,等.超高效液相色谱-四极杆串联质谱法检测饮用水中双酚A和双酚F及其氯化消毒副产物[J].中国食品卫生杂志, 2017,29(2):155-159.
相关信息
