磁分子印迹聚合物上气相色谱-质谱联用预固相萃取法测定不同类型土壤中的双酚a

A. S. Gubin, A. A. Kushnir, P. T. Sukhanov
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摘要

采用气相色谱-质谱联用双酚A (BPA)测定双酚A (BPA)的方法,采用带BPA分子印迹的吸附剂预富集(吸附剂用量为50 mg,吸附时间为10 min, pH为3,甲醇解吸)。该吸附剂单次吸附可从水溶液中提取约96%的BPA,印迹系数高,达到7.1。研究了城市化地区的土壤样品,以及沃罗涅日地区大城市以外的典型黑钙土和残余碳酸盐黑钙土。双酚a检出限为0.07 μg/kg(以干土计),校准图线性范围为0.3 ~ 35 μg/kg。双酚的测定受到石油产品污染土壤的影响,用庚烷洗涤可消除土壤污染。结果表明,土壤pH值对双酚a沿土壤剖面的迁移有显著影响。绘制了深度为1 m的土壤剖面上BPA浓度分布曲线。城市化地区土壤中最大双酚a浓度取决于该地区受聚合物废物污染的程度。在城市生活垃圾填埋场附近采集的样品中,在20 cm深度处测得最大BPA浓度(29.84 μg/kg)。在城市范围内的其他点,最高浓度在5.38 - 8.77 μg/kg之间。在沃罗涅日市以外,双酚a在碱性和残余钙质黑钙土中的迁移率增加,在50 - 80厘米的深度发现了显著的污染物浓度。该方案可用于有针对性地筛选和监测BPA含量。该方法可用于测定不同土壤类型、气象条件(降水、年温度状况)和领土污染(采样点附近存在未经批准的垃圾填埋场、城市生活垃圾填埋场、污水处理设施)的土壤层中的双酚a。
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Application of the GC-MS method in combination with preliminary solid phase extraction on a magnetic molecular imprinted polymer for the determination of bisphenol A in soils of various types
A method of gas chromatography-mass spectrometry (GC-MS) in combination with pre-concentration on a sorbent with BPA molecular imprints (dosage of sorbent — 50 mg, sorption time — 10 min, pH — 3, desorption with methanol) is used to determine bisphenol A (BPA). The sorbent extracts about 96% of BPA from aqueous solutions with a single sorption and is characterized by a high imprinting factor reaching 7.1. The samples of soils of urbanized territories, as well as typical chernozems and residual carbonate chernozems outside the large cities of the Voronezh region were studied. The limit of BPA detection was 0.07 μg/kg (in terms of dry soil), the range of the linearity of the calibration graph was 0.3 – 35 μg/kg. Determination of bisphenol is hindered by soil contamination with petroleum products, which can be eliminated by washing with heptane. It has been revealed that pH of soils has a significant effect on the BPA migration of along the soil profile. The concentration curves of the BPA distribution over the soil profile up to a depth of 1 m were plotted. The maximum BPA concentrations in the soils of urbanized territories depend on the contamination of the territory with polymer waste. The maximum BPA concentrations (29.84 μg/kg) were determined at a depth of 20 cm in samples taken near the landfill of municipal solid waste. At other points within the city limits, the maximum concentrations range within 5.38 – 8.77 μg/kg. Outside the city of Voronezh, the mobility of BPA increases in more alkaline typical and residual-calcareous chernozems and significant concentrations of the pollutant were found at a depth of 50 – 80 cm. The developed scheme can be applied to targeted screening and monitoring of the BPA content. The method can be used for BPA determination in soil horizons for various soil types, meteorological conditions (precipitation, annual temperature regime), and contamination of the territory (the presence of unauthorized landfills, MSW landfills, sewage treatment facilities near the sampling point).
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