Determination of 17 types of phthalates in drinking water by solid-phase extraction coupled with multiple reaction monitoring of gas chromatography-mass spectrometry
SHI Mengxing, YANG Yan, DU Limin
Zhengzhou Center for Disease Control and Prevention, Zhengzhou, Henan 450007, China
Abstract:Objective To determine 17 types of phthalic acid esters (PAEs) in drinking water using solid-phase extraction coupled with gas chromatography-mass spectrometry (GC-MS) in multiple reaction monitoring (MRM) mode. Methods One litre of commercially available bottled water was purified using an HLB solid-phase extraction column, and was eluted with ethyl acetate, dichloromethane and average methanol. Seventeen types of PAEs were detected using a triple quadrupole gas chromatography-mass spectrometer in MRM mode. By optimizing the temperature programming and adjusting the mass spectrometry collision energy, collection efficiency was improved and matrix interference was reduced. The precision and accuracy of this method were assessed by determining the standard curves, detection limits, quantification limits, relative standard deviations (RSD) and average spiked recovery rates for the 17 types of PAEs. Results The 17 types of PAEs showed good linear relationships between mass concentration and chromatographic peak areas in the range of 0.02 to 1.0 mg/L, with correlation coefficients all greater than 0.999 1. The detection limits ranged from 0.002 9 to 0.009 7 mg/kg, the quantification limits ranged from 0.008 7 to 0.029 1 mg/kg, the RSD ranged from 0.8% to 3.0%, and the average spiked recovery rates ranged from 88.8% to 111.8%. Conclusion Solid-phase extraction coupled with MRM of GC-MS can better determine low concentrations of PAEs in drinking water.
石梦醒, 杨妍, 杜利敏. 固相萃取气相色谱质谱法多反应监测模式检测饮用水17种邻苯二甲酸酯[J]. 预防医学, 2025, 37(1): 102-108.
SHI Mengxing, YANG Yan, DU Limin. Determination of 17 types of phthalates in drinking water by solid-phase extraction coupled with multiple reaction monitoring of gas chromatography-mass spectrometry. Preventive Medicine, 2025, 37(1): 102-108.
[1] 刘静,徐沛维,陈志健,等.人群邻苯二甲酸酯暴露水平研究综述[J].预防医学,2021,33(9):906-909,912. LIU J,XU P W,CHEN Z J,et al.The exposure levels of phthalic acid esters in population:a review[J].China Prev Med J,2021,33(9):906-909,912.(in Chinese) [2] 曹龙,张朝升,陈秋丽,等.邻苯二甲酸酯的环境污染和生态行为及毒理效应研究进展[J].生态毒理学报,2018,13(2):34-46. CAO L,ZHANG C S,CHEN Q L,et al.Progress in the study of environmental pollution and ecological behavior and toxicological effects of phthalate ester[J].Asian J Ecotoxicol,2018,13(2):34-46.(in Chinese) [3] 王芳,杨凤华,杨中荣,等.湖州市市售黄酒邻苯二甲酸酯污染健康风险评价[J].预防医学,2023,35(5):421-424. WANG F,YANG F H,YANG Z R,et al.Health risk assessment of phthalic acid esters contamination in market-available yellow rice wine in Huzhou City[J].China Prev Med J,2023,35(5):421-424.(in Chinese) [4] 国家市场监督管理总局,国家标准化管理委员会.生活饮用水标准检验方法第8部分:有机物指标:GB/T 5750.8—2023[S].2023. State Administration for Market Regulation,National Standardization Administration.Standard examination methods for drinking water—Part 8:Organic indices:GB/T 5750.8—2023[S].2023.(in Chinese) [5] 邹开贺. 自动固相微萃取-气相色谱-串联质谱法测定瓶装水中17种邻苯二甲酸酯[J].分析仪器,2024(2):42-47. ZOU K H.Determination of 17 phthalate esters in bottled waters using automatic solid-phase microextraction and gas chromatography tandem mass spectrometry[J].Anal Instrum,2024(2):42-47.(in Chinese) [6] 郑烽,郝国辉,李楠楠,等.三重四极杆气质联用仪多反应离子监测模式检测三种常见邻苯二甲酸酯[J].现代食品,2022,28(16):210-213. ZHENG F,HAO G H,LI N N,et al.Determination of three common phthalate esters by MRM of GC-MS/MS[J].Mod Food,2022,28(16):210-213.(in Chinese) [7] 国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中邻苯二甲酸酯的测定:GB 5009.271—2016[S].2016. National Health and Family Planning Commission,State Food and Drug Administration.National food safety standard—Determination of phthalates in food:GB 5009.271—2016[S].2016.(in Chinese) [8] 管悦,泮燕媚.液液萃取气相色谱-串联质谱法测定含油半固体食品中19种邻苯二甲酸酯类化合物[J].化学分析计量,2024,33(4):90-94,100. GUAN Y,PAN Y M.Determination of 19 phthalic acid esters in oily semi-solid food by liquid-liquid extraction combined with GC-MS/MS[J].Chem Anal Meterage,2024,33(4):90-94,100.(in Chinese) [9] 李申莹. 固相萃取-气相色谱质谱法同时检测水中5种塑化剂[J].化学工程师,2023,37(10):49-51. LI S Y.Simultaneous determination of five plasticizers in water by solid phase extraction GC-MS[J].Chem Eng,2023,37(10):49-51.(in Chinese) [10] 余蕾,张小毅.气相色谱-三重四极杆质谱法测定地下水中44种有机物污染物[J].岩矿测试,2021,40(3):365-374. YU L,ZHANG X Y.Determination of 44 organic pollutants in groundwater by gas chromatography-triple quadrupole mass spectrometry[J].Rock Miner Anal,2021,40(3):365-374.(in Chinese) [11] 王芳,胡明友,杨凤华,等.磁性固相萃取-气相色谱-串联质谱法测定黄酒中16种邻苯二甲酸酯[J].中国卫生检验杂志,2022,32(17):2072-2076. WANG F,HU M Y,YANG F H,et al.Determination of 16 phthalate esters in yellow rice wine by magnetic solid-phase extraction combined with gas chromatography-tandem mass spectrometry[J].Chin J Health Lab Tec,2022,32(17):2072-2076.(in Chinese)