利用PTFE管線前濃縮配合流動注入火焰式原子吸收光譜儀之連線檢驗系統進行尿液中鉛與銅之研究

On-Line PTFE Tubing Preconcentration Device Coupling with FI-FAAS for Determination of Ultra-Trace Lead and Copper in Urine

楊婷婷(Ting-Ting Yang)

指導教授 ： 黃友利

高雄醫學大學/醫學院/醫學研究所/碩士(2005年)

摘要

前濃縮技術在微量元素線上分析方法的開發上扮演相當重要的角色。利用中空管線線上前濃縮裝置結合流動注入火焰式原子吸收光譜儀(Flame atomic spectrometer, FAAS)，本研究成功地發展出人類尿液中微量鉛和銅的線上火焰式原子吸收光譜分析法。本連線方法利用具吸附金屬螯合劑之鐵氟龍(Polytetrafluoroethylene, PTFE)材質的中空管線進行前濃縮，首先將金屬螯合劑吡咯烷二硫代氨基甲酸銨(Ammonium pyrrolidine dithiocarbamate, APDC)通入PTFE管線中，使其吸附在管壁上。之後將樣品導入PTFE管線中，最後利用鹽酸當沖提液沖出管線內的待測元素，藉由攜帶溶液與霧化器的攝入吸引力，將沖提出的濃縮液導入FAAS中進行待測元素的連線偵測。本研究所建立的PTFE tubing-FI-FAAS連線方法使用0.2％（v/v）超純硝酸作為攜帶溶液，霧化器攝入最適流速設定為6.0 mL/min。本研究分析方法的驗證如下：鉛和銅的線性範圍分別為0.1-0.6 mg/L 和0.05-0.4 mg/L；偵測極限分別為25和4 mg/L；精密度（RSD％）分別小於7.5 (inter-assay, n = 5)和7.1％ (intra-assay, n = 7)；添加鉛和銅的標準液於尿液中之回收率均在100％上下。此外，利用石墨爐式原子吸收光譜法進行方法比對分析，證實本研究所建立的PTFE tubing-FI-FAAS連線方法的準確性與可靠性。

關鍵字

銅 ； 鉛 ； 尿液 ； 原子吸收光譜儀 ； 前濃縮

並列摘要

Preconcentration techniques play important roles in on-line methods development. In the present study, using a polytetrafluoroethylene (PTFE) tubing preconcentration and flow-injection flame atomic absorption spectrometric detection, we have successfully developed an analytical system for enrichment and determination of trace lead (Pb) and copper (Cu) in urine. The sample mixed with ammonium pyrrolidine dithiocarbamate (APDC) was passing through a PTFE tubing and the Pb (Ⅱ)-PDC and Cu (Ⅱ)-PDC complex were absorbed quantitatively on the tubing. The preconcentrated complex was effectively eluted by hydrochloric acid solution and introduced into the nebulizer-burner system. In this method, 0.2% (v/v) HNO3 solution was used as carrier solution and the optimal flow rate of nebulizer was set at 6.0 mL/min. The calibration curve was linear over the concentration range of 0.1-0.6 mg/L and 0.05-0.4 mg/L for Pb and Cu, respectively. The limits of detection were 25 and 4 mg/L, for lead and copper, respectively. The intra- and inter-assay for lead and copper at three levels of standard solution (0.1, 0.2 and 0.3 mg/L for lead; 0.05, 0.1 and 0.2 mg/L for copper) were less than 7.5 and 7.1%. The recoveries of lead and copper spiked in human urine samples ranged from 96.7 to 108.1% and 93-96% for Pb and Cu, respectively. Furthermore, by comparing the results obtained using the developed on-line preconcentration method and graphite furnace atomic absorption spectrometry, we found the method is reliable for the determination of lead and copper in urine.

並列關鍵字

copper ； lead ； preconcentration ； on-line ； urine ； Pb ； Cu ； FAAS ； AAS ； PTFE

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