Please wait a minute...
文章检索
预防医学  2025, Vol. 37 Issue (1): 102-108    DOI: 10.19485/j.cnki.issn2096-5087.2025.01.022
  实验技术 本期目录 | 过刊浏览 | 高级检索 |
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
石梦醒, 杨妍, 杜利敏
郑州市疾病预防控制中心,河南 郑州 450007
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
全文: PDF(925 KB)  
输出: BibTeX | EndNote (RIS)      
摘要 目的 应用固相萃取气相色谱质谱法多反应监测(MRM)模式检测饮用水中17种邻苯二甲酸酯(PAEs)。方法 取市售瓶装水水样1 L,经HLB柱固相萃取,乙酸乙酯、二氯甲烷和甲醇洗脱后,收集洗脱液。采用三重四极杆气相色谱-质谱联用仪MRM模式检测17种PAEs。通过优化程序升温、调整质谱碰撞能量等提高采集效率、减少基质干扰。绘制17种PAEs的标准曲线,计算检出限、定量限、相对标准偏差(RSD)和平均回收率,评价方法的精密度和准确度。结果 在0.02~1.0 mg/L范围内,17种PAEs质量浓度与色谱峰面积均有良好的线性关系,相关系数均>0.999 1,检出限为0.002 9~0.009 7 mg/kg,定量限为0.008 7~0.029 1 mg/kg,RSD为0.8%~3.0%,平均回收率为88.8%~111.8%。结论 采用固相萃取气相色谱质谱法MRM模式可以更好地测定饮用水中低浓度PAEs。
服务
把本文推荐给朋友
加入引用管理器
E-mail Alert
RSS
作者相关文章
石梦醒
杨妍
杜利敏
关键词 固相萃取气相色谱质谱法邻苯二甲酸酯饮用水    
AbstractObjective 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.
Key wordssolid-phase extraction    gas chromatography-mass spectrometry    phthalates    drinking water
收稿日期: 2024-07-08      修回日期: 2024-11-06      出版日期: 2025-01-10
中图分类号:  R991  
  R123  
作者简介: 石梦醒,硕士,主管技师,主要从事理化检验工作
通信作者: 杨妍,E-mail:1981915951@qq.com   
引用本文:   
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.
链接本文:  
http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2025.01.022      或      http://www.zjyfyxzz.com/CN/Y2025/V37/I1/102
[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)
[1] 赵薛飞, 王爱红, 史碧君, 谷少华, 张丹丹. 宁波市生活饮用水健康风险评估[J]. 预防医学, 2024, 36(4): 333-337.
[2] 俞莎, 徐美佳, 徐小民. 液相色谱-串联质谱法测定腌制河豚鱼中河豚毒素[J]. 预防医学, 2023, 35(7): 640-644.
[3] 王芳, 杨凤华, 杨中荣, 邵国健, 王晔. 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.
[4] 王芳, 杨凤华, 邵国健, 胡明友, 王晔. 磁性固相萃取-气相色谱-串联质谱法测定市售酒中16种邻苯二甲酸酯[J]. 预防医学, 2022, 34(8): 855-860.
[5] 周少磊, 刘波, 王鹏, 郑旭, 董静. 北京市通州区农村饮用水砷暴露健康风险评估[J]. 预防医学, 2022, 34(7): 705-709.
[6] 刘静, 徐沛维, 陈志健, 邵斌, 施长苗, 李胜, 王晓峰. 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.
[7] 廖雅芬, 叶坚, 杨业洲. 肇庆市城市饮用水化学物质健康风险评估[J]. 预防医学, 2021, 33(9): 951-954.
[8] 张力群, 刘少颖, 任韧, 何华丽. 超高效液相色谱-串联质谱法检测生活饮用水8种N-亚硝胺类化合物[J]. 预防医学, 2021, 33(8): 855-858.
[9] 吴建兵, 陈祝军, 钱志荣, 吴梅, 秦园. 连续流动注射仪测定饮用水中挥发酚的方法研究[J]. 预防医学, 2021, 33(4): 424-426.
[10] 张晓艺, 张秀尧, 蔡欣欣, 李瑞芬. 超高效液相色谱-三重四极杆质谱联用同时测定饮用水13种N-亚硝胺类消毒副产物[J]. 预防医学, 2021, 33(2): 212-216.
[11] 周继恩, 杨振清, 赵永信, 冯靓, 田春霞, 王军淋, 张晶, 韩见龙, 张念华. 气相色谱质谱联用法同时测定水中2, 4, 6-三氯酚、五氯酚、2, 4-二氯苯氧乙酸和灭草松[J]. 预防医学, 2021, 33(12): 1282-1285.
[12] 陈强, 吴位新, 王祚懿, 盛微, 何晓庆. 金华市农村居民生活饮用水卫生知识调查[J]. 预防医学, 2020, 32(4): 422-425.
[13] 郝翠萍, 刘利, 孟志敏. 焦作市城市生活饮用水卫生监测结果分析[J]. 预防医学, 2020, 32(3): 307-309.
[14] 纪律, 李启, 李伟营, 徐峻卿. 超高效液相色谱-三重四级杆质谱法测定水中二氯喹啉酸残留[J]. 预防医学, 2020, 32(12): 1283-1286.
[15] 姚建花, 邵国健, 胡明友, 刘弢, 郭和光. 顶空加盐-气相色谱电子捕获检测器法测定饮用水中11种挥发性卤代消毒副产物[J]. 预防医学, 2020, 32(11): 1185-1188.
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed