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[求助]
请教各位有用薄层色谱法检测无机盐的吗
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请教各位大侠有用薄层色谱法检测无机盐的吗？本人按照BP2016方法检测，为何重现不出来呢，连对照品也没有斑点，不知原因何在？请各位帮下忙分析下原因，谢谢。。。 Impurity A (inorganic nitrates) Thin-layer chromatography (2.2.27). Test solution If necessary, dilute the solution to be examined to a concentration of 10 g/L with anhydrous ethanol R. Reference solution Dissolve 5 mg of potassium nitrate R in 1 mL of water R and dilute to 100 mL with ethanol (96 per cent) R. PlateTLC silica gel plate R. Mobile phaseglacial acetic acid R, acetone R, toluene R (15:30:60 V/V/V). Application 10 μL. Development Over 2/3 of the plate. Drying In a current of air until the acetic acid is completely removed. Detection Spray intensively with freshly prepared potassium iodide and starch solution R; expose to ultraviolet light at 254 nm for 15 min and examine in daylight. Limit: — nitrate ion: any spot due to the nitrate ion in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with the reference solution (0.5 per cent of the content of glyceryl trinitrate calculated as potassium nitrate). |
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2楼2017-06-08 16:12:04