Division of Nano-materials Science, EcoTopia Science Institute, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603, Japan.
Talanta. 2011 Dec 15;87:24-9. doi: 10.1016/j.talanta.2011.09.022. Epub 2011 Sep 29.
A method for multielement analysis of micro-volume biological sample by inductively coupled plasma mass spectrometry (ICP-MS) with a highly efficient sample introduction system was presented. The sample introduction system was the combination of (1) an inert loop injection unit and (2) a high performance concentric nebulizer (HPCN) coupled with a temperature controllable cyclone chamber. The loop injection unit could introduce 20 μL samples into the carrier liquid flow of 10 μL min(-1) producing a stable signal for 100s without any dilution. The injection loop is continuously washed with 0.1M HNO(3) carrier solution during the measurement, thereby much improving sample throughput. The HPCN is a triple tube concentric nebulizer, which can generate fine aerosols and provide a stable and highly measurement sensitivity in ICP-MS at a liquid flow rate less than 10 μL min(-1). With the combination of the chamber heating at 60°C, the sensitivity obtained with the proposed sample introduction system at the liquid flow rate of 10 μL min(-1) was almost the same as that with a common concentric nebulizer and cyclone chamber system at the liquid flow rate of 1 mL min(-1), though the sample consumption rate of the HPCN was two orders of the magnitude lower than that of the common nebulizer. The validation of the proposed system was performed by analyzing the NIST SRM 1577b Bovine Liver. The observed values for 12 elements such as Na, P, S, K, Ca, Mn, Fe, Co, Cu, Zn, Mo, Cd were in good agreement with their certified values and information value. Satisfactory analytical results for 14 elements such as Na, Mg, P, S, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Y, Ba in Escherichia coli sample were also obtained. The proposed sample introduction system was quite effective in the cases when only micro-volume of biological sample is available.
介绍了一种采用高效进样系统的电感耦合等离子体质谱法（ICP-MS）对微体积生物样品进行多元素分析的方法。该进样系统由（1）惰性环进样单元和（2）高效同心雾化器（HPCN）与温度可控旋流室相结合而成。环进样单元可将 20μL 样品引入 10μL min(-1) 的载液流中，无需稀释即可在 100s 内产生稳定的信号。在测量过程中，进样环会连续用 0.1M HNO(3)载液溶液冲洗，从而大大提高了样品通量。HPCN 是一种三管同心雾化器，在低于 10μL min(-1)的载液流量下，可产生细小的气溶胶，并在 ICP-MS 中提供稳定且高的测量灵敏度。当与腔室加热至 60°C 相结合时，在 10μL min(-1)的载液流量下，与传统同心雾化器和旋流室系统相比，所提出的进样系统的灵敏度几乎相同，尽管 HPCN 的样品消耗率比普通雾化器低两个数量级。通过分析 NIST SRM 1577b 牛肝对该系统进行了验证。12 种元素（如 Na、P、S、K、Ca、Mn、Fe、Co、Cu、Zn、Mo、Cd）的测定值与标准值和信息值吻合良好。大肠杆菌样品中 14 种元素（如 Na、Mg、P、S、K、Ca、Cr、Mn、Fe、Ni、Cu、Zn、Y、Ba）的分析结果也令人满意。在只有少量生物样品的情况下，该进样系统非常有效。
