北京市农田回用再生水中抗生素残留分布特征研究
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- 英文论文题名：Study of concentration distribution of 12 antiboiotcis in Reclaimed Water for farmland irrigation in Beijing.
- 论文作者：李安 ; 张秀彤 ; 王冬 ; 靳欣欣 ; 满燕 ; 潘立刚
- 英文论文作者：LI An ; ZHANG Xiu-tong ; WANG Dong ; JIN Xin-xin ; MAN Yan ; PAN Li-gang ; Beijing Research Center of Agriculture Standards and Testing / Risk Assessment Lab of Agri-products Quality and Safety of Ministry of Agriculture (Beijing) / Beijing Municipal Key Laboratory of Agriculture Environment Monitoring
- 年：2015
- 作者机构：北京农业质量标准与检测技术研究中心/农业部农产品质量安全风险评估实验室(北京)/农产品产地环境监测北京市重点实验室;
- 论文关键词：抗生素 ; 超高效液相色谱串联质谱 ; 再生水 ; 固相萃取
- 英文论文关键词：Antibiotics ; UPLC-MS/MS ; Reclaimed Water ; Solid Phase Extraction
- 会议召开时间：2015-11-26
- 会议录名称：2015年水资源生态保护与水污染控制研讨会论文集
- 语种：中文
- 分类号：X703
- 学会代码：HJKP
- 会议名称：2015年水资源生态保护与水污染控制研讨会
- 会议地点：中国海南海口
- 主办单位：中国环境科学学会、哈尔滨师范大学
- 学会名称：中国环境科学学会
- 页数：8
- 文件大小：1128k
- 原文格式：D
- 会议级别：全国
摘要
采用固相萃取-超高效液相色谱-串联质谱法,在多反应监测(MRM)正离子(ESI+)模式下,建立了水体中12种抗生素的定性和定量分析方法。该方法利用HLB固相萃取小柱富集水体中的痕量抗生素,以0.1%甲酸水/乙腈为流动相,经C18色谱柱分离,采用电喷雾离子源、MRM质谱监测和ESI+扫描模式,实现了水体中12种抗生素的同时检测,此法分析速度快(8 min),线性关系良好(r2>0.99),RSD在0.63%~9.60%之间,回收率范围为70~120%,检出限在0.026~1.266 ng·L-1之间。利用该方法对北京市某再生水灌区再生水出水口、再生水灌溉渠和农田灌溉点的水样进行了抗生素残留检测,并基于采样位置分析了抗生素的空间分布特征。结果表明,主要检出了2种磺胺类抗生素(磺胺嘧啶和新诺明)、1种喹诺酮类抗生素(诺氟沙星)和2种大环内酯类抗生素(红霉素和罗红霉素),其中诺氟沙星的检出含量最高,浓度主要分布在50~150 ng·L-1范围,且灌渠中浓度要明显高于出水口。总体上再生水灌溉渠下游的抗生素浓度水平要明显低于上游再生水出水口,但诺氟沙星的浓度在灌渠中端最高,因此存在再生水灌渠受二次污染而导致下游抗生素浓度升高的情况。
In this study, a qualitative and quantitative analysis method of twelve antibiotics in water was established by solid phase extraction(SPE)- ultra high performance liquid chromatography(UPLC)- tandem mass spectrometry(MS), using multiple reaction monitoring(MRM) positive ion mode. The antiobiotics with trace amount in water samples were enriched by HLB solid phase extraction cartridge, and then separated under the mobile phase of 0.1% formic acid / acetonitrile using C18 column. The targets was then turned into fragments by electrospray ionization source in positive scanning mode monitored by MRM mode. The 12 kinds of antibiotics were simultaneous determined using the established method, with short analysis time(8 min), good linearity(r2 > 0.99), high precision(0.63%-9.60%), acceptable spiked recoveries(70 ~ 120%) and low detection limits(0.026 ~ 1.266 ng·L-1). This method was applied in the analysis of reclaimed water from an irrigation area of Beijing. Samples collected at the outlet, recycled water irrigation canal, and farmland were analyzed. Results showed that five antibiotics(sulfadiazine, sulfamethoxazole, norfloxacin, erythrocin, and roxithromycin) were detected in all of the samples. Large amout of norfloxacin was detected, with the concentration between 31 ~ 748 ng·L-1. Generally, the level of antibiotic concentration at the downstream of reclaimed water irrigation cannal was significantly lower than the upstream(reclaimed water outlet). However, the amount of norfloxacin in irrigation canals was higher than in water outlet. This may be caused by the secondary pollution of the canals.
In this study, a qualitative and quantitative analysis method of twelve antibiotics in water was established by solid phase extraction(SPE)- ultra high performance liquid chromatography(UPLC)- tandem mass spectrometry(MS), using multiple reaction monitoring(MRM) positive ion mode. The antiobiotics with trace amount in water samples were enriched by HLB solid phase extraction cartridge, and then separated under the mobile phase of 0.1% formic acid / acetonitrile using C18 column. The targets was then turned into fragments by electrospray ionization source in positive scanning mode monitored by MRM mode. The 12 kinds of antibiotics were simultaneous determined using the established method, with short analysis time(8 min), good linearity(r2 > 0.99), high precision(0.63%-9.60%), acceptable spiked recoveries(70 ~ 120%) and low detection limits(0.026 ~ 1.266 ng·L-1). This method was applied in the analysis of reclaimed water from an irrigation area of Beijing. Samples collected at the outlet, recycled water irrigation canal, and farmland were analyzed. Results showed that five antibiotics(sulfadiazine, sulfamethoxazole, norfloxacin, erythrocin, and roxithromycin) were detected in all of the samples. Large amout of norfloxacin was detected, with the concentration between 31 ~ 748 ng·L-1. Generally, the level of antibiotic concentration at the downstream of reclaimed water irrigation cannal was significantly lower than the upstream(reclaimed water outlet). However, the amount of norfloxacin in irrigation canals was higher than in water outlet. This may be caused by the secondary pollution of the canals.
引文
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[2]Yi L,Jiao W,Chen X,et al.An overview of reclaimed water reuse in China.Journal of Environment Science[J].Journal of Environmental Sciences,2011,23(10):1585-1593.
[3]尹世洋,吴文勇,刘洪禄,等.北京市农业再生水利用现状与监测[J].北京水务,2012(A01):54-58.
[4]陈卫平,张炜铃,潘能,等.再生水灌溉利用的生态风险研究进展[J].环境科学,2012,1(12):4070-4080.
[5]王冉,刘铁铮,王恬.抗生素在环境中的转归及其生态毒性[J].生态学报,2006,01期(1):265-270.
[6]Hong P Y,Al-Jassim N,Ansari M I,et al.Environmental and Public Health Implications of Water Reuse:Antibiotics,Antibiotic Resistant Bacteria,and Antibiotic Resistance Genes[J].Antibiotics,2013,2(3):367-399.
[7]王丽平,顾国平,章明奎.抗生素残留对农产品安全与生态环境的影响[J].安徽农学通报,2007,02:74-76.
[8]段晓洁.喹诺酮类抗生素在蔬菜体内迁移和积累的研究[D].安徽农业大学,2012.
[9]吴小莲,莫测辉,严青云,等.东莞市蔬菜基地蔬菜中喹诺酮类抗生素污染特征及健康风险[J].中国环境科学,2013,5:910-916.
[10]胡洪营,吴乾元,黄晶晶,等.再生水水质安全评价与保障原理[M].北京:科学出版社,2011:14.
[11]徐维海,张干,邹世春,等.典型抗生素类药物在城市污水处理厂中的含量水平及其行为特征[J].环境科学,2007,28:1779-1783.
[12]张娣,王懿萱,牛红云,等.纳米Fe3O4/H2O2降解诺氟沙星[J].环境科学,2011,10:2943-2948.
[13]Haque M M,Muneer M.Photodegradation of norfloxacin in aqueous suspensions of titanium dioxide[J].Journal of Hazardous Materials,2007,145(1-2):51–57.
[14]郭文渊.大环内酯类抗生素的研究进展[J].医学信息,2013,16:665-665.
[15]唐才明,黄秋鑫,余以义,等.污泥和沉积物中微量大环内酯类、磺胺类抗生素、甲氧苄胺嘧啶和氯霉素的测定[J].分析化学,2009,8:1119-1124.
[16]阮悦斐,陈继淼,郭昌胜,等.天津近郊地区淡水养殖水体的表层水及沉积物中典型抗生素的残留分析[J].农业环境科学学报,2011,12:2586-2593.