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请教毛细管电泳间接紫外法测K+Na6Ca2+Mg2+四种离子的方法

毛细管电泳(CE)

  • 最近找了一篇文献,按文中方法操作,但重复不出来,迷惑不解中!不知有没有高人知道好的方法,请指点一二,在下不胜感激,有文献就更好了,我的邮箱是ddssll007@163.com,再次谢过!
  • 该帖子已被版主-nini2006加5积分,加2经验;加分理由:发帖奖励
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  • ericwong

    第1楼2013/05/16

    楼主说说在文献中看到的方法,不然别人不知道楼主用过什么方法,也不好提出其它方法

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  • 金樱子

    第2楼2013/05/16

    我用的方法见附件,请多指教!

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  • 金樱子

    第3楼2013/05/16

    采用方法如下:采用电压进样(5 kV,8 s),紫外检测器检测,检测波长为214 nm.分离电压为20 kV,操作温度为25℃,每次实验前将毛细管用0·1 mol/LNaOH、二次蒸馏水各清洗5 min,运行电解质溶液清洗10 min.两次运行之间用运行电解质溶液冲洗2 min.为保证分析结果的重现性,运行电解质溶液每运行3次后要更新.所有溶液在进样前均用
    0·45μm微孔滤膜过滤,再超声脱气5 min以除去气泡.

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  • nini2006

    第4楼2013/05/16

    同一个实验室同一个人不同时间做的结果都有可能会有很大差异,更何况你这是重复中文文章上人家的工作呢?要重复别人的工作基本上所有条件都要重新优化的。

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  • nini2006

    第5楼2013/05/16

    这里有两篇文献可供你参考:
    1、http://apps.webofknowledge.com.ezproxy.cityu.edu.hk/full_record.do?product=WOS&search_mode=GeneralSearch&qid=1&SID=Y1HPNMICFjDa5E6A99K&page=2&doc=19&cacheurlFromRightClick=no

    Determination of Na+, K+, Mg2+ and Ca2+ in mixtures of seawater and formation water by capillary electrophoresis

    Author(s): Tangen, A (Tangen, A); Lund, W (Lund, W); Frederiksen, RB (Frederiksen, RB)
    Source: JOURNAL OF CHROMATOGRAPHY A Volume: 767 Issue: 1-2 Pages: 311-317 DOI: 10.1016/S0021-9673(97)00007-1 Published: APR 11 1997
    Times Cited: 32 (from Web of Science)
    Cited References: 31 [ view related records ] Citation MapCitation Map

    Abstract: A method has been developed for the determination of Na+, K+, Mg2+ and Ca2+ in mixtures of seawater and formation water from oil wells in the North Sea by capillary electrophoresis with indirect UV detection. The carrier electrolyte contained 5.0 mM 4-methylbenzylamine (UVCAT-1), 6.5 mM alpha-hydroxyisobutyric acid (HIBA), 6.2 mM 18-crown-6 and 25% (v/v) methanol. Baseline separation was achieved for concentrations below 70 ppm Na+, 20 ppm K+, 50 ppm Mg2+, 30 ppm Ca2+, 10 ppm Sr2+ and 10 ppm Ba2+. The limits of detection were 0.14 ppm Na+, 0.15 ppm K+, 0.08 ppm Mg2+, 0.08 ppm Ca2+, 0.18 ppm Sr2+ and 0.15 ppm Ba2+. The accuracy was checked by analysis of a reference water sample. The precision was better than 3.0%.

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  • nini2006

    第6楼2013/05/16

    2 http://apps.webofknowledge.com.ezproxy.cityu.edu.hk/full_record.do?product=WOS&search_mode=GeneralSearch&qid=1&SID=Y1HPNMICFjDa5E6A99K&page=2&doc=14&cacheurlFromRightClick=no

    Quantitative determination of K+, NH4+, Na+, Ca2+ and Mg2+ cations in secreted human sweat by capillary zone electrophoresis
    Author(s): Terasawa, J (Terasawa, J); Mitsuya, K (Mitsuya, K); Ishii, A (Ishii, A); Tsuda, T (Tsuda, T)
    Source: BUNSEKI KAGAKU Volume: 50 Issue: 12 Pages: 813-817 Published: DEC 2001
    Times Cited: 9 (from Web of Science)
    Cited References: 19 [ view related records ] Citation MapCitation Map

    Abstract: Cations in human insensible perspiration were analyzed by capillary zone electrophoresis. A simple sampling method from the skin surface of the forefinger of a hand was demised. After washing the forefinger with tap water and then distilled water for 10 s, 40 mul of a 10% ethanol aqueous solution kept in a small vial (0.6 ml) was allowed to contact the treated forefinger for 3 minutes. The sweat sample was then analyzed by capillary zone electrophoresis. A mixture of 5.0 mmol l(-1) copper(II) acetate, 10 mmol l(-1) ethylendiamine and 1.0 mmol l(-1) 18-crown-6-ether at pH 6.5 was selected as the optimum medium for capillary zone electrophoresis. Six cations {Rb+ (I.S.), K+, NH4+, Na+, Ca2+ and Mg2+} were completely separated in less than 3 min, and detected with indirect UV detection at 230 nm. Sweat samples were collected from seven volunteers. They were healthy males (n = 4) and females (n = 3), aged 21 similar to 25 years. The mean values of the cation concentrations were K+ = 39.9 mM, Na+ = 54.0 mM, Ca2+ = 5.49 mM, Mg2+ = 1.67 mM, NH4+ = 5.13 mM. It shoud be noted that the concentration of K+ in secreted sweat is much higher than that in serum.

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  • nini2006

    第7楼2013/05/16

    最后提醒你一句:很多SCI文章都是水货,更不要说中文文献了。呵呵~

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  • 金樱子

    第8楼2013/05/17

    非常感谢nini2006!
    谈到国人的科学研究真是痛心疾首啊,不过不知道蚕蛾3号是否也是满载H2O上天的?!

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  • nini2006

    第9楼2013/06/09

    哎,这个可带不了H2O啊,几条人命在上面啊。

    金樱子(v2728738) 发表:非常感谢nini2006!
    谈到国人的科学研究真是痛心疾首啊,不过不知道蚕蛾3号是否也是满载H2O上天的?!

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  • ericwong

    第10楼2013/06/13

    楼主的实验怎么样了?

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