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违禁药物作为一种新型污染物得到了环境科学界的广泛关注.本文根据国内外已有研究,比较了污水样的前处理条件如SPE柱和水样pH值、冲洗、酸化及复溶过程.结果表明,对实际污水样的前处理应将样品pH值调为2,选用Oasis MCX柱,无需除杂质的冲洗和氮吹过程的酸化步骤,因两种上机测定方法 HILIC-UPLC-MS/MS和C18-UPLC-MS/MS不同而分别选择200μL乙腈和100μL乙腈+100μL 5 mmol·L~(-1)乙酸铵复溶.通过比较HILIC法和C18法的保留时间及检出限、定量限、回收率和基质效应等方法评价指标,确定污水样的测定应选用C18-UPLC-MS/MS.最后,将优化后的测定方法用于分析北京市12家污水处理厂的进、出水样,验证了方法的可靠性,为违禁药物的污水流行病学研究和环境风险评价奠定了基础.
As a new type of pollutant, the banned drug has attracted a great deal of attention from the environmental science community.According to the existing researches at home and abroad, this paper compares the wastewater pretreatment conditions such as pH value, rinsing, acidification and reconstitution process of SPE column and water sample. The results show that for the actual wastewater sample preparation, the pH of the sample should be adjusted to 2 and the Oasis MCX column should be used. No impurity removal and acidification steps are required. Two methods for on-board determination of HILIC-UPLC-MS / 200 μL acetonitrile and 100 μL acetonitrile + 100 μL 5 mmol·L -1 ammonium acetate were used to reconstitute MS and C18-UPLC-MS / MS, respectively.Comparing the retention time and the detection limit of HILIC and C18, Limit, recoveries and matrix effects and other methods to evaluate the indicators to determine the determination of sewage samples should be used C18-UPLC-MS / MS.Finally, the optimized determination method for the analysis of Beijing’s 12 sewage treatment plants into and out of water The results validated the reliability of the method and laid the foundation for epidemiological studies and environmental risk assessment of illicit drugs.