高级搜索

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

,  ,  ,  ,  , 

downloadPDF

上一篇

下一篇

刘娴静, 梁存珍, 肖本益, 杨悦颜, 韩超, 赵飞. 高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品[J]. 环境化学, 2021, (2): 549-558. doi: 10.7524/j.issn.0254-6108.2019092706
引用本文: 刘娴静, 梁存珍, 肖本益, 杨悦颜, 韩超, 赵飞. 高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品[J]. 环境化学, 2021, (2): 549-558. doi: 10.7524/j.issn.0254-6108.2019092706
shu
LIU Xianjing, LIANG Cunzhen, XIAO Benyi, YANG Yueyan, HAN Chao, ZHAO Fei. Simultaneous determination of 26 pharmaceuticals and personal care products (PPCPs) in water using solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2021, (2): 549-558. doi: 10.7524/j.issn.0254-6108.2019092706
Citation: LIU Xianjing, LIANG Cunzhen, XIAO Benyi, YANG Yueyan, HAN Chao, ZHAO Fei. Simultaneous determination of 26 pharmaceuticals and personal care products (PPCPs) in water using solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2021, (2): 549-558. doi: 10.7524/j.issn.0254-6108.2019092706
shu

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

  • 1. 北京工业大学环境与能源工程学院, 北京, 100124;

  • 2. 北京石油化工学院环境工程系, 北京, 102617;

  • 3. 中国科学院生态环境研究中心, 北京, 100085

    • 通讯作者: 梁存珍, E-mail: liangcunzhen@bipt.edu.cn ; 
  • 基金项目:

    国家自然科学基金（41730749）资助.

Simultaneous determination of 26 pharmaceuticals and personal care products (PPCPs) in water using solid-phase extraction and liquid chromatography-tandem mass spectrometry

  • 1. College of Environmental and Energy Engineering, Beijing University of Technology, Beijing, 100124, China;

  • 2. Department of Environmental Engineering, Beijing Institute of Petrochemical Technology, Beijing, 102617, China;

  • 3. Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

    • Corresponding author: LIANG Cunzhen, liangcunzhen@bipt.edu.cn ; 
  • Fund Project: Supported by National Natural Science Foundation of China (41730749)

  • 摘要: 通过优化固相萃取条件和高效液相色谱-串联质谱参数，建立了可以同时检测地表水和地下水中26种典型药物及个人护理品（pharmaceuticals and personal care products，PPCPs），包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7，利用HLB固相萃取柱对水样中PPCPs进行富集，以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相，甲醇和含0.5 mmol·L-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱，采用多反应监测的质谱扫描模式（MRM）分析测定.26种PPCPs的检出限为0.007—1.78 ng·L-1，定量限为0.02—5.68 ng·L-1，回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度，结果表明，地表水中PPCPs的含量普遍高于地下水，磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高，检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L-1.
    Abstract: An analytical method was developed for the determination of 26 pharmaceuticals and personal care products (PPCPs) by solid-phase extraction (SPE) followed liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Water samples were concentrated with HLB cartridge at pH=7. Gradient elution was performed using methanol and 0.005% formic acid water in positive mode, and methanol and 0.5 mmol·L-1 ammonium acetate in negative mode. The mass spectrometric acquisition was carried out by multiple reaction monitoring (MRM) mode. The limits of detection (LOD) and quantitation (LOQ) for the 26 PPCPs were 0.007—1.78 ng·L-1 and 0.02—5.68 ng·L-1. The recoveries for the 26 PPCPs were in the range of 52.28%—115.24%. The method was successfully applied to investigate occurrences of persistent PPCPs in surface water and groundwater of the Chaobai River. The result revealed that the concentration of PPCPs in the surface water was higher than those in the groundwater. Moreover, the concentration of sulfamethoxazole (147.83 ng·L-1), sulpiride (52.48 ng·L-1), caffeine (78.35 ng·L-1), carbamazepine (166.58 ng·L-1) and ibuprofen (30.63 ng·L-1) were higher than other PPCPs.
  • 加载中
  • [1] XU M, HUANG H, LI N, et al. Occurrence and ecological risk of pharmaceuticals and personal care products (PPCPs) and pesticides in typical surface watersheds, China[J]. Ecotoxicology and Environmental Safety, 2019, 175(15):289-298.
    [2] LI Z, ZHENG T, LI M, et al. Organic contaminants in the effluent of Chinese wastewater treatment plants[J]. Environmental Science and Pollution Research, 2018, 25(27):26852-26860.
    [3] LIU X, ZHANG G, LIU Y, et al. Occurrence and fate of antibiotics and antibiotic resistance genes in typical urban water of Beijing, China[J]. Environmental Pollution, 2019, 246:163-173.
    [4] HONG Y, SHARMA V K, CHIANG P C, et al. Fast-target analysis and hourly variation of 60 pharmaceuticals in wastewater using UPLC-high resolution mass spectrometry[J]. Arch Environ Contam Toxicol, 2015, 69(4):525-534.
    [5] GROS M, RODR GUEZ-MOZAZ S, BARCEL D. Rapid analysis of multiclass antibiotic residues and some of their metabolites in hospital, urban wastewater and river water by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry[J]. Journal of Chromatography A, 2013, 1292(16):173-188.
    [6] KIM C, RYU H D, CHUNG E G, et al. A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water:Sample preparation, liquid chromatography, and mass spectrometry[J]. J Environ Manage, 2018, 217(1):629-645.
    [7] 张志超, 程和发. 环境介质中喹诺酮类抗生素的前处理与检测方法研究进展[J]. 环境化学, 2019, 38(1):1-22.

    ZHANG Z C, CHENG H F. Recent development in sample pretreatment and detection methods for the determination of quinolones in environmental matrices[J]. Environmental Chemistry, 2019, 38(1):1-22(in Chinese).

    [8] 殷哲云, 闵露娟, 金立涛, 等. HPLC-MS/MS测定3类污水处理厂污泥及污水中的8种药物[J]. 环境化学, 2018, 37(8):1720-1727.

    YIN Z R, MIN L J, JIN L T, et al. HPLC-MS/MS determination of eight PPCPs in sewage and sludge from three types of sewage treatment plants[J]. Environmental Chemistry, 2018, 37(8):1720-1727(in Chinese).

    [9] 丁紫荣, 贺德春, 万大娟, 等. 高效液相色谱-串联质谱法同时检测地表水中13种药物及个人护理品[J]. 环境工程学报, 2015, 9(5):2291-2296.

    DING Z R, HE D C, WAN D J, et al. Determination of thirteen pharmaceutical and personal care products in surface water by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Environmental Engineering, 2015, 9(5):2291-2296(in Chinese).

    [10] 陆静, 陈练, 付善良, 等. 高效液相色谱-三重四极杆串联质谱测定环境水样中19种个人护理品[J]. 环境化学, 2019, 38(8):1930-1940.

    LU J, CHEN L, FU S L, et al. Determination of 19 personal care products in environmental water samples by high performance liquid chromatography mass spectrometry[J]. Environmental Chemistry, 2019, 38(8):1930-1940(in Chinese).

    [11] LIU J L, WONG M H. Pharmaceuticals and personal care products (PPCPs):A review on environmental contamination in China[J]. Environment International, 2013, 59:208-224.
    [12] PENG Y, FANG W, KRAUSS M, et al. Screening hundreds of emerging organic pollutants (EOPs) in surface water from the Yangtze River Delta (YRD):Occurrence, distribution, ecological risk[J]. Environmental Pollution, 2018, 241:484-493.
    [13] LUO Y, GUO W, NGO H H, et al. A review on the occurrence of micropollutants in the aquatic environment and their fate and removal during wastewater treatment[J]. Science of the Total Environment, 2014, 473/474:619-641.
    [14] 王大鹏, 张娴, 颜昌宙. 高效液相色谱串联质谱法测定污水污泥中4种磺胺类药物及其乙酰化代谢物[J]. 环境化学, 2018, 37(10):2143-2151.

    WNAG D P, ZHANG X, YAN C Z. Determination of four sulfonamides and their corresponding acetyl metabolites in wastewater and sludge by high performance liquid chromatography tandem mass spectrometry[J]. Environmental Chemistry, 2018, 37(10):2143-2151(in Chinese).

    [15] 冉韵竹, 齐维晓, 李静, 等. 超高效液相色谱-串联质谱法同时测定水中13种药品与个人护理品[J]. 环境化学, 2018, 37(2):255-263.

    RAN Y Z, QI W X, LI J, et al. Simultaneous determination of 13 pharmaceuticals and personal care products in water using UPLC-MS/MS[J]. Environmental Chemistry, 2018, 37(2):255-263(in Chinese).

    [16] LI W, SHI Y, GAO L, et al. Occurrence of antibiotics in water, sediments, aquatic plants, and animals from Baiyangdian Lake in North China[J]. Chemosphere, 2012, 89(11):1307-1315.
    [17] DORIVAL-GARC A N, ZAFRA-G MEZ A, CANTARERO S, et al. Simultaneous determination of 13 quinolone antibiotic derivatives in wastewater samples using solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry[J]. Microchemical Journal, 2013, 106:323-333.
    [18] KIM C, RYU H D, CHUNG E G, et al. A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water:Sample preparation, liquid chromatography, and mass spectrometry[J]. Journal of Environmental Management, 2018, 217:629-645.
    [19] ZHOU L J, YING G G, LIU S, et al. Simultaneous determination of human and veterinary antibiotics in various environmental matrices by rapid resolution liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Journal of Chromatography A, 2012, 1244(12):123-138.
    [20] PETROVIĆ M, HERNANDO M D, D AZ-CRUZ M S, et al. Liquid chromatography-tandem mass spectrometry for the analysis of pharmaceutical residues in environmental samples:A review[J]. Journal of Chromatography A, 2005, 1067(1):1-14.
    [21] GMEZ M J, PETROVIĆ M, FERN NDEZ-ALBA A R, et al. Determination of pharmaceuticals of various therapeutic classes by solid-phase extraction and liquid chromatography-tandem mass spectrometry analysis in hospital effluent wastewaters[J]. Journal of Chromatography A, 2006, 1114(2):224-233.
    [22] GROS M, RODR GUEZ-MOZAZ S, BARCEL D. Rapid analysis of multiclass antibiotic residues and some of their metabolites in hospital, urban wastewater and river water by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry[J]. Journal of Chromatography A, 2013, 1292:173-188.
    [23] SUI Q, HUANG J, DENG S, et al. Rapid determination of pharmaceuticals from multiple therapeutic classes in wastewater by solid-phase extraction and ultra-performance liquid chromatography tandem mass spectrometry[J]. Chinese Science Bulletin, 2009, 54(24):4633-4643.
    [24] USEPA, 2007. Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS[S]. Method 1694.
    [25] 柯润辉, 蒋愉林, 黄清辉, 等. 上海某城市污水处理厂污水中药物类个人护理用品(PPCPs)的调查研究[J]. 生态毒理学报, 2014, 9:1146-1155. KE R H, JIANG Y L, HUANG Q H, et al. Investigative screening of pharmaceuticals in a municipal wastewater treatment plant in Shanghai[J]. Asian Journal of Ecotoxicology, 2014

    , 9(6):1146-1155(in Chinese).

    [26] ZHOU H, WU C, HUANG X, et al. Occurrence of selected pharmaceuticals and caffeine in sewage treatment plants and receiving Rivers in Beijing, China[J]. Water Environment Research A Research Publication of the Water Environment Federation, 2010, 82(11):2239-2248.
    [27] WANG J, WANG S. Removal of pharmaceuticals and personal care products (PPCPs) from wastewater:A review[J]. Journal of Environmental Management, 2016, 182:620-640.
    [28] DAI G, WANG B, HUANG J, et al. Occurrence and source apportionment of pharmaceuticals and personal care products in the Beiyun River of Beijing, China[J]. Chemosphere, 2015, 119(119C):1033-1039.
    [29] 吴苗苗. 再生水回灌过程中典型磺胺类抗生素的行为特征研究[D]. 北京:清华大学, 2015. WU M. The behavior of typical sulfanomidesin soil by groundwater recharge with reclaimed water[D]. Beijing:Tsinghua University, 2015(in Chinese).
    [30] 李建忠. 典型内分泌干扰物在土壤中迁移转化规律研究[D]. 北京:清华大学, 2013. LI J Z. Study on the migration and transformation of the typical endocrine disrupting chemicals in soil[D]. Beijing:Tsinghua University, 2013(in Chinese).
  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  2628
  • HTML全文浏览数:  2628
  • PDF下载数:  68
  • 施引文献:  0
出版历程
  • 收稿日期:  2019-09-27

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

    通讯作者: 梁存珍, E-mail: liangcunzhen@bipt.edu.cn ; 
  • 1. 北京工业大学环境与能源工程学院, 北京, 100124;
  • 2. 北京石油化工学院环境工程系, 北京, 102617;
  • 3. 中国科学院生态环境研究中心, 北京, 100085
  • 收稿日期:  2019-09-27
基金项目:

国家自然科学基金（41730749）资助.

摘要: 通过优化固相萃取条件和高效液相色谱-串联质谱参数，建立了可以同时检测地表水和地下水中26种典型药物及个人护理品（pharmaceuticals and personal care products，PPCPs），包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7，利用HLB固相萃取柱对水样中PPCPs进行富集，以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相，甲醇和含0.5 mmol·L-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱，采用多反应监测的质谱扫描模式（MRM）分析测定.26种PPCPs的检出限为0.007—1.78 ng·L-1，定量限为0.02—5.68 ng·L-1，回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度，结果表明，地表水中PPCPs的含量普遍高于地下水，磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高，检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L-1.

English Abstract

    全文HTML

参考文献 (30)

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心