High-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine
A high-performance liquid chromatography, propyl ethylenediamine technology, applied in the field of high-performance liquid chromatography analysis, can solve the problems of poor method reproducibility, poor accuracy and sensitivity, poor accuracy, etc., and achieves accurate method, high sensitivity, good reproducibility
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Embodiment 1
[0045] Example 1: N 1 ,N 1 - Diisopropylethylenediamine standard curve drawing
[0046] Take N 1 ,N 1- About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 20ml measuring bottle, and dilute with diluent To the mark, as N1,N1-diisopropylethylenediamine standard stock solution; take the appropriate amount of the above-mentioned standard stock solution precisely, and quantitatively dilute with the above-mentioned diluent to make each 1ml contain about 0.4μg, 0.8μg, 4μg, 8μg, 12μg linear solution;
[0047] Measure 1ml of each of the above linear solutions, put them in 5ml measuring bottles, add 2ml of 0.05mol / L sodium carbonate solution, add 1ml of derivatization reagent, place in a 50oC water bath for 30 minutes, cool, and then dilute to the mark with diluent. Precisely measure 10 μl each of the derivatized linear solu...
Embodiment 2
[0048] Example 2: N 1 ,N 1 - Determination of detection limit and limit of quantification of diisopropylethylenediamine.
[0049] Take N 1 ,N 1 - About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 20ml measuring bottle, and dilute with diluent to scale, as N 1 ,N 1 -Diisopropylethylenediamine limit stock solution; measure the above limit stock solution, dilute step by step with diluent to obtain limit solution, measure each 1ml of the above limit solution, put in 5ml measuring bottle respectively, add 0.05mol / Add 2ml of L sodium carbonate solution, add 1ml of derivatization reagent 2,4-dinitrofluorophenylacetonitrile solution (1%, V / V), place in 50oC water bath for 30 minutes, cool, and then dilute to the mark with diluent. Precisely measure 10 μl each of the derivatized limiting solutions, inject them into a li...
Embodiment 3
[0050] Example 3: N 1 ,N 1 - Determination of recovery rate of diisopropylethylenediamine
[0051] Take N 1 ,N 1 - About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 100ml measuring bottle, dilute with diluent to scale, as N 1 ,N 1 -Diisopropylethylenediamine standard solution.
[0052] Take an appropriate amount of the test product (equivalent to 16 mg of acotiamide hydrochloride), accurately weigh it, put it in 10 20ml measuring bottles, add diluent to dissolve, and add 1ml N to 3 of them. 1 ,N 1 - Diisopropylethylenediamine standard solution, 3 of which added 2ml N 1 ,N 1 -Diisopropylethylenediamine standard solution, 3 of which were added with 4ml N1,N1-diisopropylethylenediamine standard solution, and the last one was not added with N 1 ,N 1 -Diisopropylethylenediamine standard solution, then dilute to ...
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