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月下飞雪

金虫 (小有名气)

[求助] 请问大家烷基磷酸酯跑TLC板时用什么显色剂合适

如题,化合物如图

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hongqiangaa

新虫 (小有名气)

2楼2012-10-08 15:03:04
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月下飞雪

金虫 (小有名气)

引用回帖:
2楼: Originally posted by hongqiangaa at 2012-10-08 15:03:04
碘熏试试

有没有专属性显色剂呢?
3楼2012-11-05 10:02:32
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netscaner

木虫 (正式写手)

【答案】应助回帖

这个也许可以在荧光下看暗斑点。
以下虽说可以显磷酸酯,但是磷钼酸是一个通用显色剂,不算专属。
Ammonium molydbate
For detection of phosphoric acid derivatives
Solution I: 1M perchloric acid in water/acetone (1:1)
Solution II: ammonium molybdate soln: 5g (NH4)6Mo7O24.4 H2O in 35ml semi-conc. Nitric acid and 65ml water.
Solution III: Tin(II) chloride soln: 0.5g SnCl2.2 H2O in 100ml 0.5M hydrochloric acid:
Dry developed chromatogram and heat to 60 C
Hydrolyse di- and triphosphates by spraying perchloric acid (solution I) onto the warm plate. After spraying 2 times, dry plate slowly at 50 C. Amidophosphates might not be decomposed.
In any case, spray the still warm plate with ammonium molybdate solution (solution II)
Then spray the still wet plate with tin (II) chloride solution (solution III)
Results: Phosphates appear as blue to blue-green spots. Polyphosphates can also be detected by dipping the plates in a solution of ammonium molybdate (1g) dissolved in water (8ml) and perchloric acid (3ml, ca. 70%),filled up to 100ml with acetone. Then phosphates appear as yellow-green spots on a blue background. Also see Molybdenum blue reaction according to Dittmer and Lester.
天道酬勤!
4楼2012-11-05 15:47:41
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