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摘要:
当前对抗生素滥用监管及其研究正在加强，近年来中国主要水域中抗生素均有不同程度的检出，地表水及地下水中抗生素的污染状况持续受到关注。因进入环境中的抗生素种类繁多、结构复杂，一般实验室难以实现同时分析多种类抗生素。本文在哈尔滨市共采集地下水样品26组，采样范围包括人口密集、工业生产、农畜业等生活生产地区。利用超高效液相色谱-三重四极杆串联质谱联用技术分析了样品中的磺胺类、喹诺酮类、大环内酯类、β-内酰胺类、四环素类、林可酰胺类等6大类共29种典型抗生素含量，研究了哈尔滨市地下水中典型抗生素的检出及分布状况。结果表明：①哈尔滨市地下水中6大类典型抗生素均有不同程度检出，其中以磺胺类、喹诺酮类、大环内酯类、四环素类为主，检出率分别为61.5%、46.2%、42.3%、38.5%；②哈尔滨市地下水检出的抗生素含量范围在0.02~612ng/L之间，其中磺胺噻唑、磺胺嘧啶、林可霉素检出的最高浓度超过100ng/L，相比于国内外部分地区（如中国北京、天津，西班牙巴塞罗那）喹诺酮类整体含量偏低；③检出抗生素含量较高的采样点位主要分布在城市的中部、南部和东部地区，这些区域也是该市人口相对密集区，且附近普遍分布有制药厂、家禽牲畜养殖厂、城市排污口等。由此揭示了哈尔滨市城市地下水中抗生素分布特征受人类生产生活活动影响且具有明显的相关性。
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关键词:
- 地下水 /
- 抗生素 /
- 喹诺酮 /
- 空间分布 /
- 超高效液相色谱-三重四极杆串联质谱法
Abstract:BACKGROUND At present, the supervision of antibiotic abuse and its research is being strengthened. In recent years, antibiotics have been detected in varying degrees in water in central China. This reinforces the concern of the pollution of antibiotics in surface and groundwater.
OBJECTIVES To investigate the distribution characteristics of 29 antibiotics in groundwater in Harbin.
METHODS A total of 26 groups of groundwater samples were collected in Harbin, and the sampling scope included habitation and production areas such as densely populated, industrial production, agricultural districts and animal husbandry. The ultra-performance liquid chromatography-triple quadrupole mass spectrometry method was used to analyze 29 kinds of antibiotics covering six types, including sulfonamides, quinolones, macrolides, β-lactams, tetracyclines, and lincosamides.
RESULTS Antibiotics in the groundwater of Harbin were mainly composed of sulfonamides, quinolones, macrolides and tetracyclines and the detection rates were 61.5%, 46.2%, 42.3% and 38.5%, respectively. The content of antibiotics detected ranged from 0.02 to 681ng/L, and the highest contents of sulfathiazole, sulfadiazine, and lincomycin were more than 100ng/L. The average content of quinolones was low compared with some domestic and international areas (such as Beijing, Tianjin, and Barcelona). Sampling sites with higher antibiotic levels were mainly found in the central, southern and eastern regions of the city. These areas are also relatively densely populated and are generally distributed around pharmaceutical factories, urban sewage outlets, and poultry and livestock farms.
CONCLUSIONS The distribution characteristics of antibiotics in groundwater in Harbin are strongly related to the impact of human production and living activities.
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表 1 标准品信息
Table 1. Information of standard materials
标准品类别 标准品名称 《化学文摘》登记号(CAS No.) 浓度(μg/mL) 不确定度或纯度(%) 磺胺类(SAs) 磺胺醋酰 144-80-9 99.80 ±1.42 磺胺氯哒嗪 80-32-0 99.96 ±1.41 磺胺嘧啶 68-35-9 100.2 ±1.08 磺胺间二甲氧嘧啶 122-11-2 99.99 ±1.12 磺胺邻二甲氧嘧啶 2447-57-6 99.91 ±1.40 磺胺甲基嘧啶 127-79-7 100.1 ±1.42 磺胺对甲氧嘧啶 651-06-9 99.96 ±1.41 磺胺二甲嘧啶 57-68-1 99.60 ±1.03 磺胺甲二唑 144-82-1 99.99 ±1.12 磺胺甲基异噁唑 723-46-6 99.96 ±1.41 磺胺甲氧哒嗪 80-35-3 100.0 ±1.02 磺胺间甲氧嘧啶 1220-83-3 99.96 ±1.41 磺胺苯吡唑 526-08-9 99.99 ±1.42 磺胺吡啶 144-83-2 99.60 ±1.42 磺胺噻唑 72-14-0 100.0 ±1.01 磺胺二甲异噁唑 127-69-5 100.5 ±1.42 喹诺酮类(QNs) 奥比沙星 113617-63-3 纯品 97.5 恩诺沙星 93106-60-6 纯品 99.9 环丙沙星 93107-08-5 纯品 92.3 洛美沙星 98079-52-8 纯品 99.4 氧氟沙星 82419-36-1 纯品 95.7 诺氟沙星 70458-96-7 纯品 97.3 林可酰胺类(LCMs) 林可霉素 7179-49-9 纯品 99.6 四环素类(TCs) 四环素 64-75-5 纯品 96.2 土霉素 2058-46-0 纯品 96.0 强力霉素 24390-14-5 纯品 99.3 β-内酰胺类(PNCs) 阿莫西林 61336-70-7 纯品 98.7 大环内酯类(MLs) 红霉素 114-07-8 纯品 95.0 罗红霉素 80214-83-1 纯品 96.2 内标 磺胺甲基嘧啶-D4 1020719-84-9 100.0 ±3.0 强力霉素-D3 N/A 纯品 97.0 氧氟沙星-D3 1173147-91-5 100.0 ±3.0 替代物 磺胺嘧啶-D4 1020719-78-1 纯品 98.0 
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表 2 29种抗生素检出限、加标回收率、平行样品相对偏差
Table 2. Detection of limit, spiked recovery, relative deviation of 29 antibiotics
抗生素名称 检出限(ng/L) 空白加标平均回收率(%) 样品1 (H01) 含量(ng/L) 样品2 (H15) 含量(ng/L) 样品加标平均回收率(%) 平行样品相对偏差(%) 奥比沙星 0.025 83.8 ND ND 76.3 12.3 恩诺沙星 0.123 112.6 ND ND 114.7 10.4 环丙沙星 0.169 98.7 ND ND 82.4 10.4 洛美沙星 0.095 97.5 ND ND 93.8 3.6 诺氟沙星 0.137 103.7 ND ND 88.2 5.9 氧氟沙星 0.020 111.3 ND ND 76.9 14.8 磺胺二甲嘧啶 0.003 85.4 0.054 0.064 67.4 18.3 磺胺嘧啶 0.021 78.4 ND ND 72.9 7.9 磺胺噻唑 0.006 78.1 ND ND 69.2 6.4 磺胺氯哒嗪 0.013 70.9 ND ND 89.9 12.5 磺胺甲氧哒嗪 0.026 107.9 ND ND 92.7 19.3 磺胺间二甲氧嘧啶 0.007 80.7 ND ND 110.3 6.3 磺胺二甲异噁唑 0.008 79.0 ND ND 72.1 8.9 磺胺甲嘧啶 0.004 60.1 ND ND 62.9 10.3 磺胺醋酰 0.047 88.6 ND ND 83.5 15.6 磺胺甲塞二唑 0.007 81.0 ND ND 107.3 17.2 磺胺吡啶 0.016 83.8 ND ND 65.9 11.2 磺胺苯吡唑 0.004 73.4 ND ND 89.0 8.3 磺胺对甲氧嘧啶 0.019 77.9 ND ND 93.7 9.4 磺胺甲基异噁唑 0.022 68.2 ND ND 62.9 15.6 磺胺间甲氧嘧啶 0.032 85.8 ND ND 99.2 7.3 磺胺邻二甲氧嘧啶 0.017 70.1 ND ND 72.8 9.5 林可霉素 0.007 108.0 ND 0.231 115.9 8.4 强力霉素 0.052 88.6 ND ND 118.7 13.1 四环素 0.158 46.7 ND ND 52.4 9.8 土霉素 0.091 53.3 ND ND 50.8 10.6 阿莫西林 0.041 54.4 ND ND 63.4 17.3 红霉素 0.040 64.0 0.513 0.592 59.2 16.7 罗红霉素 0.023 59.5 ND ND 52.7 18.4 注：“ND”表示未检出。
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表 3 哈尔滨地区与国内外其他地区地下水抗生素检出率对比
Table 3. Comparison of detection rate of antibiotics in different areas of Harbin City and other areas
抗生素类别 各地区抗生素检出率(%) 哈尔滨(26个采样点) 北京(19个采样点) 江汉平原(27个采样点) 华北及西南地区(74个采样点) 西班牙(巴塞罗那31个采样点) 美国(18个州47个采样点) 美国(养殖场附近17个采样点) 磺胺类 61.5 78.9 72.0 67.5 100 23.4 47.1 喹诺酮类 46.2 100 78.9 37.3 100 ND - 大环内酯类 42.3 ND 100 - 100 ND 47.1 四环素类 38.5 47.3 73.7 58.4 23 ND - 林可酰胺类 19.2 - 100 63.5 100 5.4 - 氯霉素类 - - - 29.7 ND ND - β-内酰胺类 7.7 ND - - 15 - 5.8 数据来源 本文研究 文献[22] 文献[31] 文献[32] 文献[9] 文献[7] 文献[8] 注：“ND”表示未检出；“-”表示文献中未提及。
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表 4 哈尔滨市地下水抗生素浓度检测结果
Table 4. Detected antibiotics concentration in groundwater of Harbin City
抗生素类别 抗生素名称 检出浓度范围(ng/L) 检出浓度平均值(ng/L) 磺胺类 磺胺甲二唑 0.05~12.4 2.39 磺胺嘧啶 0.09~68.6 29.9 磺胺噻唑 1.55~612.0 176.0 磺胺甲嘧啶 0.08~15.3 4.01 磺胺苯吡唑 0.19~2.61 1.12 磺胺对甲氧嘧啶 0.29~4.35 2.33 磺胺吡啶 0.34~0.43 0.38 磺胺甲异噁唑 1.24~6.95 3.19 磺胺间甲氧嘧啶 0.13~1.94 1.02 喹诺酮类 氧氟沙星 0.02~0.05 0.04 恩诺沙星 0.19~0.64 0.29 环丙沙星 0.59~1.06 0.82 诺氟沙星 0.15~0.89 0.51 林可酰胺类 林可霉素 0.23~158.0 44.5 β-内酰胺类 阿莫西林 0.91~1.47 1.19 大环内酯类 红霉素 0.24~23.3 3.88 罗红霉素 0.16~1.58 0.91 四环素类 强力霉素 0.35~3.91 2.14
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