Method for detecting 1, 3-dihydroxyacetone and related impurities
A technology of dihydroxyacetone and a detection method, applied in the field of analysis and detection, can solve the problems of inaccurate results, inability to be decomposed, unstable detection results and the like
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Embodiment 1
[0033] Example 1 Chromatographic method construction
[0034] 1. Prepare the sample and spiking solution:
[0035] Standard addition solution: respectively weigh glycerol, glyceraldehyde, 1,3-dihydroxyacetone and add water to dissolve into a mixed solution containing 0.25 mg of glycerol, 0.5 mg of glyceraldehyde, and 50 mg of 1,3-dihydroxyacetone per 1 ml.
[0036] 2. Detect the solution prepared in 1 with the following chromatographic parameters
[0037] Column: Carbomix Ca-NP 10:8% 7.8×300mm, 10μm
[0038] Water was used as the mobile phase; the column temperature was 60°C; the flow rate was 0.5 ml per minute; the detector temperature was 55°C; the injection volume was 20 μl.
[0039] 3 Detection effect
[0040] Chromatogram( figure 1 ) shows that the chromatographic conditions meet the verification requirements. The peaks of glyceraldehyde, glycerol and 1,3-dihydroxyacetone appeared successively. The separation degree of 1,3-dihydroxyacetone and glycerol was 2.12, and ...
Embodiment 2
[0041] Embodiment 2 chromatographic accuracy verification
[0042] 1 Prepare the solution with water as the diluent
[0043] Mixed reference solution: Take appropriate amounts of glycerol and glyceraldehyde reference substances, dissolve in water and dilute to make a mixed solution containing 0.25 mg of glycerol and 0.25 mg of glyceraldehyde per 1 ml.
[0044]50% recovery rate solution: take appropriate amounts of 1,3-dihydroxyacetone, glycerol and glyceraldehyde, dissolve in water and dilute to prepare a solution containing 50 mg of 1,3-dihydroxyacetone, 0.125 mg of glycerol and 0.125 mg of glyceraldehyde per 1 ml Mix the solution and get it. Prepare 3 servings in the same way
[0045] 100% recovery rate solution: take appropriate amounts of 1,3-dihydroxyacetone, glycerol, and glyceraldehyde, dissolve in water and dilute to prepare a solution containing 50 mg of 1,3-dihydroxyacetone, 0.25 mg of glycerol, and 0.25 mg of glyceraldehyde per 1 ml. Mix the solution and get it. ...
Embodiment 3
[0056] Example 3 chromatographic repeatability verification
[0057] 1. Use water as a solution to prepare a repeatable solution:
[0058] Take appropriate amounts of 1,3-dihydroxyacetone, glycerol and glyceraldehyde, dissolve in water and dilute to make a mixed solution containing 50 mg of 1,3-dihydroxyacetone, 0.25 mg of glycerol and 0.25 mg of glyceraldehyde per 1 ml. Prepare 6 servings in the same way
[0059] 2. Detect with the chromatographic conditions recorded in Example 1, and the detection results are as shown in Tables 3 to 4:
[0060] table 3
[0061]
[0062] Table 4
[0063]
[0064] It can be seen from Tables 3-4 that in the 6 repeatable solutions, the average content of glycerol is 0.49%, and the content RSD is 0.20%; the average content of glyceraldehyde is 0.54%, and the content RSD is 0.83%; indicating that the method has good repeatability.
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