固相萃取—超高效液相色谱串联质谱法对杭州市不同水环境中13种痕量药物残留状况的检测及分析
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摘要
本文应用固相萃取和超高效液相色谱-串联质谱(UPLC-MS/MS)技术,建立了同时定量检测水中13种目标药物残留的方法。建立的方法满足日常分析需要,同时也成功地应用在了杭州市不同水环境中目标药物残留状况的调查中。
从医院→污水处理厂→地表水分别检测和分析13种目标药物的浓度空间分布特征上看：
医院出水检出药物的总浓度在3083.4-5878.3ng/L之间。检出频率最高的几种药物是甲氧苄胺嘧啶、红霉素、诺氟沙星、氧氟沙星和阿替洛尔,但是不同药物在不同医院的污水残留浓度相差甚大,尤其是喹诺酮类药物诺氟沙星和氧氟沙星在所有医院中的检出浓度相对较高,总浓度在9000ng/L左右,超过了国外一些学者预测的对地表水菌群产生影响的无效浓度3000ng/L (Predicted No-effect Concentration)。
由于药物性质和污水处理厂进水性质的不同,污水处理厂的去除率和进水中药物的组成也存在差异。在所调查的污水处理厂中,PPCPs并不能完全去除,这一结果表明污水处理厂的处理工艺主要侧重于常规水体污染物的去除,并没有考虑到痕量药物的去除。
钱塘江流域18个监测点中目标药物残留总浓度为13.8ng/L～1189.3ng/L。其中抗生素占很高比例,检出浓度和比例最高的抗生素类药物是喹诺酮类药物诺氟沙星。钱塘江中上游药物残留相对较低,下游由于人类活动相对集中,药物残留浓度较高,这也证明地表水中的药物残留在很大程度上受人类活动的影响。
在所有的水环境中,检出药物的组成均有所不同,浓度在ng/L-μg/L之间,与其他药物相比,抗生素类药物尤其是诺氟沙星的检出率和浓度相对较高,证实了该类药物的广泛来源和使用率。在后续试验阶段,需要更进一步加强对该类药物的调查和研究。
A method for the simultaneous determination of thirteen target pharmaceuticals residues in water samples using solid phase extraction (SPE) and ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established and successfully applied in the survey of 13 pharmaceuticals in different water samples in Hangzhou.
Different pharmaceuticals composition was found in the hospital wastewater samples with the total pharmaceuticals concentration 3083.4-5878.3ng/L. PEN-G and NAP were below method detection limits in all of the hospital wastewater analyzed. TRI, ERY, NOR, OFL and ATEN were the most frequently detected pharmaceuticals, whereas, varied among the hospitals. Total concentration of quinolones including NOR and OFL was about 9000ng/L in all hospital samples, higher than the other pharmaceuticals detected, exceeding the no-effect concentration of total quinolones for surface water organisms predicted by some academics.
The removal efficiencies of WWTPs and pharmaceutical compositions varied between the WWTPs. The results from the WWTPs showed that treatment process of WWTPs mainly focused on the removal of conventional pollutants, not taking into account the removal of trace chemicals.
Total concentrations of the target drugs residue occurred at the levels ranging from 13.8ng/L to 1189.3ng/L in 18 monitoring points of Qiantang River. A high proportion of antibiotics was measured in all samples, and the most detected antibiotics were fluoroquinolone NOR. Drugs also were found relatively low in the upper reaches of the river, compared with lower reaches. Higher concentrations of drug residues were found in lower reaches, which also proved that the drug residues in surface water were largely affected by human activities.
Concentrations of pharmaceuticals were at different levels from ng/L toμg/L in all the samples, with higher concentrations of NOR, especially. The results suggested the widespread source and use of NOR in this region. It needed to be further investigated in subsequent research for this kind of pharmaceuticals.
从医院→污水处理厂→地表水分别检测和分析13种目标药物的浓度空间分布特征上看：
医院出水检出药物的总浓度在3083.4-5878.3ng/L之间。检出频率最高的几种药物是甲氧苄胺嘧啶、红霉素、诺氟沙星、氧氟沙星和阿替洛尔,但是不同药物在不同医院的污水残留浓度相差甚大,尤其是喹诺酮类药物诺氟沙星和氧氟沙星在所有医院中的检出浓度相对较高,总浓度在9000ng/L左右,超过了国外一些学者预测的对地表水菌群产生影响的无效浓度3000ng/L (Predicted No-effect Concentration)。
由于药物性质和污水处理厂进水性质的不同,污水处理厂的去除率和进水中药物的组成也存在差异。在所调查的污水处理厂中,PPCPs并不能完全去除,这一结果表明污水处理厂的处理工艺主要侧重于常规水体污染物的去除,并没有考虑到痕量药物的去除。
钱塘江流域18个监测点中目标药物残留总浓度为13.8ng/L～1189.3ng/L。其中抗生素占很高比例,检出浓度和比例最高的抗生素类药物是喹诺酮类药物诺氟沙星。钱塘江中上游药物残留相对较低,下游由于人类活动相对集中,药物残留浓度较高,这也证明地表水中的药物残留在很大程度上受人类活动的影响。
在所有的水环境中,检出药物的组成均有所不同,浓度在ng/L-μg/L之间,与其他药物相比,抗生素类药物尤其是诺氟沙星的检出率和浓度相对较高,证实了该类药物的广泛来源和使用率。在后续试验阶段,需要更进一步加强对该类药物的调查和研究。
A method for the simultaneous determination of thirteen target pharmaceuticals residues in water samples using solid phase extraction (SPE) and ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established and successfully applied in the survey of 13 pharmaceuticals in different water samples in Hangzhou.
Different pharmaceuticals composition was found in the hospital wastewater samples with the total pharmaceuticals concentration 3083.4-5878.3ng/L. PEN-G and NAP were below method detection limits in all of the hospital wastewater analyzed. TRI, ERY, NOR, OFL and ATEN were the most frequently detected pharmaceuticals, whereas, varied among the hospitals. Total concentration of quinolones including NOR and OFL was about 9000ng/L in all hospital samples, higher than the other pharmaceuticals detected, exceeding the no-effect concentration of total quinolones for surface water organisms predicted by some academics.
The removal efficiencies of WWTPs and pharmaceutical compositions varied between the WWTPs. The results from the WWTPs showed that treatment process of WWTPs mainly focused on the removal of conventional pollutants, not taking into account the removal of trace chemicals.
Total concentrations of the target drugs residue occurred at the levels ranging from 13.8ng/L to 1189.3ng/L in 18 monitoring points of Qiantang River. A high proportion of antibiotics was measured in all samples, and the most detected antibiotics were fluoroquinolone NOR. Drugs also were found relatively low in the upper reaches of the river, compared with lower reaches. Higher concentrations of drug residues were found in lower reaches, which also proved that the drug residues in surface water were largely affected by human activities.
Concentrations of pharmaceuticals were at different levels from ng/L toμg/L in all the samples, with higher concentrations of NOR, especially. The results suggested the widespread source and use of NOR in this region. It needed to be further investigated in subsequent research for this kind of pharmaceuticals.
引文
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