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Ultrasonication extraction and solid phase extraction clean-up for determination of US EPA 16 priority pollutant polycyclic aromatic hydrocarbons in soils by reversed-phase liquid chromatography with ultraviolet absorption detection

机译:超声波萃取和固相萃取净化-反相液相色谱-紫外吸收检测法测定土壤中美国EPA 16优先污染物多环芳烃

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A method using ultrasonication extraction and solid phase extraction (SPE) clean-up for determination of US EPA 16 priority pollutant polycyclic aromatic hydrocarbons (PAHs) in soils by reversed-phase liquid chromatography (RP-LC) with ultraviolet (UV) absorption detection was studied. Separation and detection of the 16 PAHs were completed in 31 min by RP-LC with a Cls column (Bakerbond PAH 6 PLUS 125 x 3.0 i.d. mm or Phenomenex ENVIROSEP-PP 125 x 3.2 i.d. mm), acetonitrile water gradient elution and UV absorption detection. The detection limits, for a 10 mu l of solution injection, determined at 254 nm were less than 1 mu g/ml, except for acenaphthene, which was 1.05 mu g/ml. Because individual PAHs are present in soils at the ng/g level or below and few sample matrices can be analyzed directly without serious interference, efficient extraction, preconcentration and clean-up of PAHs from the samples are indispensable prior to the determination of the PAHs. Several organic solvents were tested for extraction of the PAHs from soils, and ultrasonication extraction was used for the extraction in acetone of the 16 PAHs in soils. Several SPE procedures were tested and compared, and Supelco 6 mi LC-18 SPE cartridge and acetone:tetrahydrofuran (THF) = 1:1 eluant were used for the preconcentration and clean-up of the 16 PAHs in the soil. The method was successfully applied to determine the 16 PAHs in the soil sampled from an industrial land in the UK. (C) 1998 Elsevier Science B.V. [References: 28]
机译:采用超声提取和固相萃取(SPE)净化的方法,采用反相液相色谱(RP-LC)和紫外(UV)吸收检测法测定土壤中的US EPA 16优先污染物多环芳烃(PAHs)。研究。通过带有Cls色谱柱(Bakerbond PAH 6 PLUS 125 x 3.0 id mm或Phenomenex ENVIROSEP-PP 125 x 3.2 id mm),乙腈水梯度洗脱和UV吸收检测的RP-LC在31分钟内完成16种PAH的分离和检测。 。对于10μl溶液注射液,在254 nm处测定的检出限小于1μg/ ml,但啶为1.05μg/ ml。由于土壤中存在的单个PAH浓度为ng / g或以下,并且几乎没有样品基质可以直接分析而没有严重干扰,因此在测定PAH之前,必须从样品中进行有效的提取,预浓缩和净化PAH。测试了几种有机溶剂从土壤中提取PAHs的方法,超声提取用于从丙酮中提取土壤中16种PAHs的方法。测试和比较了几种SPE程序,并使用Supelco 6 mi LC-18 SPE柱和丙酮:四氢呋喃(THF)= 1:1洗脱液对土壤中的16种PAH进行了预浓缩和净化。该方法已成功应用于测定英国工业用地土壤中的16种多环芳烃。 (C)1998 Elsevier Science B.V. [参考:28]

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