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SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素

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吕凯, 刘晓薇, 邓呈逊, 郑坤, 李兰兰, 史江红, 郭伟. SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素[J]. 环境化学, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
引用本文: 吕凯, 刘晓薇, 邓呈逊, 郑坤, 李兰兰, 史江红, 郭伟. SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素[J]. 环境化学, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
shu
LYU Kai, LIU Xiaowei, DENG Chengxun, ZHENG Kun, LI Lanlan, SHI Jianghong, GUO Wei. Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS[J]. Environmental Chemistry, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
Citation: LYU Kai, LIU Xiaowei, DENG Chengxun, ZHENG Kun, LI Lanlan, SHI Jianghong, GUO Wei. Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS[J]. Environmental Chemistry, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
shu

SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素

  • 1. 合肥工业大学资源与环境工程学院, 合肥, 230009;

  • 2. 合肥工业大学纳米矿物与污染控制安徽普通高校重点实验室, 合肥, 230009;

  • 3. 合肥学院生物与环境工程系, 合肥, 230022;

  • 4. 南方科技大学环境科学与工程学院广东省土壤与地下水防控及修复重点实验室, 深圳, 518055

    • 通讯作者: 刘晓薇, E-mail: liuxw@hfut.edu.cn ; 
  • 基金项目:

    国家自然科学基金（51609058），中国博士后基金（2016M602009），合肥学院科研发展基金（18ZR03ZDA），国家重点研发计划（2018YFC1801603）和深圳市科技创新委员会（CYJ20160301114534506）.

Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS

  • 1. School of Resources and Environmental Engineering, Hefei University of Technology, Hefei, 230009, China;

  • 2. Key Laboratory of Nanominerals and Pollution Control of Anhui Higher Education Institutes, Hefei University of Technology, Hefei, 230009, China;

  • 3. China Department of Biological and Environmental Engineering, Hefei University, Hefei, 230022, China;

  • 4. Guangdong Provincial Key Laboratory of Soil and Groundwater Pollution Control, School of Environmental Science and Engineering, Southern University of Science and Technology, Shenzhen, 518055, China

    • Corresponding author: LIU Xiaowei, liuxw@hfut.edu.cn ; 
  • Fund Project: Supported by the National Natural Science Foundation of China (51609058), the China Postdoctoral Science Foundation (2016M602009) the Scientific Research Development Fund from Hefei University (18ZR03ZDA), the National Key R&D Program of China (2018YFC1801603), and the Shenzhen Municipal Science and Technology Innovation Committee Project (CYJ20160301114534506).

  • 摘要: 针对磺胺类、喹诺酮类、四环素类、大环内酯类共14种典型抗生素，建立了水和沉积物中固相萃取-高分离快速液相色谱-串联质谱（SPE-RRLC-MS/MS）前处理方法和仪器检测方法.14种抗生素在5—100 μg·L-1范围内线性良好，相关系数r ≥ 0.990.优化后的前处理方法采用乙腈/0.1 mol·L-1 EDTA-Mcllvaine（1∶1，V/V）作为沉积物样品中目标抗生素的提取剂，甲醇/丙酮（85∶15，V/V）作为固相萃取柱的洗脱液.表层水中14种抗生素的加标回收率为56%—117%，相对标准偏差（n=3）为0.10%—12%；沉积物中14种抗生素的加标回收率为57%—127%，相对标准偏差（n=3）为0.10%—25%.表层水和沉积物中抗生素的方法检出限分别为0.18—5.88 ng·L-1和0.25—2.94 ng·g-1.该方法用于检测合肥市南淝河表层水和沉积物中的抗生素，5种抗生素被检出，浓度范围分别为32—308 ng·L-1和2.70—329 ng·g-1.
    Abstract: A solid phase extraction-high separation rapid liquid chromatography-tandem mass spectrometry (SPE-RRLC-MS/MS) method was developed to simultaneously determinate 14 typical antibiotics including sulfonamides, quinolones, tetracycline and macrolides in water and sediments. The pretreatment process was improved to obtain high recoveries. The mixture of acetonitrile/0.1 mol·L-1 EDTA-Mcllvaine (1:1, V/V) was selected as the extraction solvent of antibiotics in the sediment samples. The mixture of methanol/acetone (85:15, V/V) was used to elute these target antibiotics. The results showed that the linear range of the 14 antibiotics was between 5-100 μg·L-1(r ≥ 0.990). The recovery and relative standard deviation (RSD, n=3) of 14 antibiotics in surface water were 56%-117% and 0.10%-12%, respectively. The recovery and RSD (n=3) of 14 antibiotics in sediments were 57%-127% and 0.10%-25%, respectively. The detection limit of these antibiotics in surface water and sediments ranged from 0.18 ng·L-1 to 5.88 ng·L-1 and from 0.25 ng·g-1 to 2.94 ng·g-1, respectively. The method was applied to detect antibiotics in the Nanfei River, Hefei City. Five antibiotics were detected in surface water and sediments in the ranges of 32-308 ng·L-1 and 2.70-329 ng·g-1, respectively.
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  • [1] 方媛瑗, 丁惠君. 抗生素的生态毒性效应研究进展[J]. 环境科学与技术, 2018, 41(5):102-110.

    FANG Y Y, DING H J. Advance in ecological toxicity of antibiotics[J]. Environmental Science & Technology, 2018, 41(5):102-110(in Chinese).

    [2] YING G G, HE L Y, YING A J, et al. China must reduce its antibiotic use[J]. Environmental Science & Technology, 2017, 51(3):1072-1073.
    [3] QIAO M, YING G G, SINGER A C, et al. Review of antibiotic resistance in China and its environment[J]. Environmental International, 2018, 110:160-172.
    [4] 张国栋, 董文平, 刘晓晖, 等. 我国水环境中抗生素赋存、归趋及风险评估研究进展[J]. 环境化学, 2018, 37(7):1491-1500.

    ZHANG G D, DONG W P, LIU X H, et al. Occurrence, fate and risk assessment of antibiotics in water environment of China[J]. Environmental Chemistry, 2018, 37(7):1491-1500(in Chinese).

    [5] ZHANG Q Q, YING G G, PAN C G, et al. Comprehensive evaluation of antibiotics emission and fate in the river basins of china:source analysis, multimedia modeling, and linkage to bacterial resistance[J]. Environmental Science & Technology, 2015, 49(11):6772-6782.
    [6] JOHNSON, A C, KELLER V, DUMONT E, et al. Assessing the concentrations and risks of toxicity from the antibiotics ciprofloxacin, sulfamethoxazole, trimethoprim and erythromycin in European rivers[J]. Science of the Total Environment, 2015, 511:747-755.
    [7] VERRAES C, VAN B S, VAN M E, et al. Antimicrobial resistance in the food chain:A review[J]. International Journal of Environmental Research and Public Health, 2013, 10(7):2643-2669.
    [8] 戴晓虎, 薛勇刚, 刘华杰, 等. 基于固相萃取及高效液相色谱-荧光检测分析的污泥中氟喹诺酮类抗生素研究方法的开发[J]. 环境科学, 2016, 37(4):1553-1561.

    DAI X H, XUE Y G, LIU H J, et al. Development of determination method of fluoroquinolone antibiotics in sludge based on solid phase extraction and HPLC-fluorescence detection analysis[J]. Environmental Science, 2016, 37(4):1553-1561(in Chinese).

    [9] 宋淑敏, 张翔宇, 周佳虹, 等. 超高效液相色谱串联质谱法同时测定城市污水处理厂污泥中12种抗生素[J]. 环境化学, 2017, 36(9):1923-1931.

    SUN S M, ZHANG X Y, ZHOU J H, et al. Simultaneous determination of 12 antibiotics in sewage sludge by ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(9):1923-1931(in Chinese).

    [10] 董恒涛, 姚劲挺, 郝红元, 等. 超高效液相色谱三重四极杆质谱联用法测定地表水中14种喹诺酮类抗生素残留[J]. 环境化学, 2018, 37(6):1436-1439.

    DONG H T, YAO J T, HAO H Y, et al. Determination of 14 quinolones residues in surface water by UHPLC-MS/MS[J]. Environmental Chemistry, 2018, 37(6):1436-1439(in Chinese).

    [11] 张金, 宗栋良, 常爱敏, 等. 水环境中典型抗生素SPE-UPLC-MS/MS检测方法的建立[J]. 环境化学, 2015, 34(8):1446-1452.

    ZHANG J, ZONG D L, CHANG A M, et al. Determination of common antibiotics in aquatic environment by solid- phase extraction and ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)[J]. Environmental Chemistry, 2015, 34(8):1446-1452(in Chinese).

    [12] 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.
    [13] LUO Y, XU L, MICHAL R, et al. Occurrence and transport of tetracycline, sulfonamide, quinolone, and macrolide antibiotics in the Haihe River basin, China[J]. Environmental Science & Technology, 2011, 45(5):1827-1833.
    [14] 张猛, 胡翔. SPE-HPLC法测定城市污水中8种四环素类抗生素[J]. 环境科学与技术, 2018, 41(7):141-144.

    ZHANG M, HU X. Determination of eight tetracyclines in municipal wastewater by SPE-HPLC[J]. Environmental Science & Technology, 2018, 41(7):141-144(in Chinese).

    [15] 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 Y, 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).

    [16] TLILI I, CARIA G, OUDDANE B, et al. Simultaneous detection of antibiotics and other drug residues in the dissolved and particulate phases of water by an off-line SPE combined with on-line SPE-LC-MS/MS:Method development and application[J]. Science of the Total Environment, 2016, 563(564):424-433.
    [17] BLACKWELLl P A, HOLTEN L H C, Ma H P, et al. Ultrasonic extraction of veterinary antibiotics from soils and pig slurry with SPE clean-up and LC-UV and fluorescence detection[J]. Talanta, 2004, 64(4):1058-1064.
    [18] LILLENBERG M, YURCHENKO S, KIPPER K, et al. Simultaneous determination of fluoroquinolones, sulfonamides and tetracyclines in sewage sludge by pressurized liquid extraction and liquid chromatography electrospray ionization-mass spectrometry[J]. Journal of Chromatography A, 2009, 1216(32):5949-5954.
    [19] MONTESDEOCA E, SARAH, SOSA F, et al. Combination of microwave-assisted micellar extraction with liquid chromatography tandem mass spectrometry for the determination of fluoroquinolone antibiotics in coastal marine sediments and sewage sludges samples[J]. Biomedical Chromatography, 2015, 26(1):33-40.
    [20] LIU J L, WONG M H. Pharmaceuticals and personal care products (PPCPs):A review on environmental contamination in China[J]. Environment International, 2013, 59C(3):208-224.
    [21] BU Q, WANG B, HUANG J, et al. Pharmaceuticals and personal care products in the aquatic environment in China:A review[J]. Journal of Hazardous Material, 2013, 262, 189-211.
    [22] LI S, SHI W, LIU W, et al. A duodecennial national synthesis of antibiotics in China'ds major rivers and seas (2005-2016)[J]. Science of Total Environment, 2018, 615, 906-917.
    [23] 黄秋鑫, 陈琼, 雷敏, 等. 同位素内标稀释高效液相色谱-质谱法同时测定水中多种痕量抗生素[J]. 环境化学, 2016, 35(7):1493-1499.

    HUANG Q X, CHEN Q, LEI M, et al. Simultaneous determination of trace antibiotics in surface water by isotope-diluted high performance liquid chromalography-mass spectrometry[J]. Environmental Chemistry, 2016, 35(7):1493-1499(in Chinese).

    [24] CHANG X, MEYER M T, LIU X, et al. Determination of antibiotics in sewage from hospitals, nursery and slaughter house, wastewater treatment plant and source water in Chongqing region of Three Gorge Reservoir in China[J]. Environmental Pollution, 2010, 158(5):1444-1450.
    [25] 国家统计局城市社会经济调查司.中国城市统计年鉴-2017[Z]. 北京:中国统计出版社, 2017. Department of urban socio-economic survey, national bureau of statistics. China city statistical yearbook-2017[Z]. Beijing:China Statistics Press, 2017(in Chinese).
    [26] 秦晓栋, 刘晓薇, 王慧, 等. 基于MIKE11模型的南淝河及其支流内分泌干扰风险评价与调控[J]. 环境科学学报, 2018, 38(7):2884-2893

    QIN X D, LIU X W, WANG H, et al. Risk of Endocrine disruption in the Nanfei River and its tributaries assessed and controlled using MIKE11[J]. 2018, 38(7):2884-2893(in Chinese).

    [27] 中华人民共和国水利部. 中国河流泥沙公报[R]. 北京:中国水利水电出版社, 2017. Ministry of Water Resources of the People'ds Republic of China. China river sediment bulletin[R]. Beijing:China Water & Power Press, 2017(in Chinese).
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  • 收稿日期:  2018-12-29
吕凯, 刘晓薇, 邓呈逊, 郑坤, 李兰兰, 史江红, 郭伟. SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素[J]. 环境化学, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
引用本文: 吕凯, 刘晓薇, 邓呈逊, 郑坤, 李兰兰, 史江红, 郭伟. SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素[J]. 环境化学, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
shu
LYU Kai, LIU Xiaowei, DENG Chengxun, ZHENG Kun, LI Lanlan, SHI Jianghong, GUO Wei. Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS[J]. Environmental Chemistry, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
Citation: LYU Kai, LIU Xiaowei, DENG Chengxun, ZHENG Kun, LI Lanlan, SHI Jianghong, GUO Wei. Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS[J]. Environmental Chemistry, 2019, (11): 2415-2424. doi: 10.7524/j.issn.0254-6108.2018122904
shu

SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素

    通讯作者: 刘晓薇, E-mail: liuxw@hfut.edu.cn ; 
  • 1. 合肥工业大学资源与环境工程学院, 合肥, 230009;
  • 2. 合肥工业大学纳米矿物与污染控制安徽普通高校重点实验室, 合肥, 230009;
  • 3. 合肥学院生物与环境工程系, 合肥, 230022;
  • 4. 南方科技大学环境科学与工程学院广东省土壤与地下水防控及修复重点实验室, 深圳, 518055
  • 收稿日期:  2018-12-29
基金项目:

国家自然科学基金（51609058），中国博士后基金（2016M602009），合肥学院科研发展基金（18ZR03ZDA），国家重点研发计划（2018YFC1801603）和深圳市科技创新委员会（CYJ20160301114534506）.

摘要: 针对磺胺类、喹诺酮类、四环素类、大环内酯类共14种典型抗生素，建立了水和沉积物中固相萃取-高分离快速液相色谱-串联质谱（SPE-RRLC-MS/MS）前处理方法和仪器检测方法.14种抗生素在5—100 μg·L-1范围内线性良好，相关系数r ≥ 0.990.优化后的前处理方法采用乙腈/0.1 mol·L-1 EDTA-Mcllvaine（1∶1，V/V）作为沉积物样品中目标抗生素的提取剂，甲醇/丙酮（85∶15，V/V）作为固相萃取柱的洗脱液.表层水中14种抗生素的加标回收率为56%—117%，相对标准偏差（n=3）为0.10%—12%；沉积物中14种抗生素的加标回收率为57%—127%，相对标准偏差（n=3）为0.10%—25%.表层水和沉积物中抗生素的方法检出限分别为0.18—5.88 ng·L-1和0.25—2.94 ng·g-1.该方法用于检测合肥市南淝河表层水和沉积物中的抗生素，5种抗生素被检出，浓度范围分别为32—308 ng·L-1和2.70—329 ng·g-1.

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