HPLC-RID (High Performance Liquid Chromatography-Resin Identifier) purity detection method of erythritol disulfate

Abstract

The invention provides an HPLC-RID (High Performance Liquid Chromatography-Resin Identifier) purity detection method of erythritol disulfate. The HPLC-RID is adopted for detection. A blank solvent, a standard substance solution and a sample solution are prepared respectively, the blank solvent is used for detecting a solvent peak, the standard substance solution is used for detecting the retention time of the erythritol disulfate, and the purity of the erythritol disulfate can be obtained through integral calculation of the peak area of each substance in the sample solution and integral calculation of the peak area of the erythritol disulfate. The method is easy to operate and high in accuracy, and data has good repeatability and application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of analysis and detection, and in particular to an HPLC-RID purity detection method for erythrose disulfate. Background Art

[0002] Erythrose disulfate is a white powder that is insoluble in water and miscible with acetonitrile. It is an important electrolyte additive and can be used as an additive for lithium-ion battery electrolytes.

[0003] Currently, there is no report on the HPLC-RID purity detection method for erythrose disulfate. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide an HPLC-RID purity detection method for erythrose disulfate with simple operation, high accuracy and good repeatability.

[0005] The technical solution of the present invention is achieved as follows: the present invention provides an HPLC-RID purity detection method for erythrose disulfate, which uses a liquid chromatograph to perform purity detection on erythrose disulfate.

[0006] The detection method of the present invention comprises the following steps:

[0007] Prepare blank solvent: take appropriate amount of acetonitrile and set aside;

[0008] Prepare standard solution: weigh 1g of erythrose disulfate standard into a clean container, pipette 25ml of acetonitrile to dissolve it to obtain standard solution, set aside;

[0009] Prepare sample solution: weigh 1g of erythrose disulfate sample into a clean container, pipette 25ml of acetonitrile to dissolve it to obtain sample solution for later use;

[0010] Injection: Weigh 10 μL of blank solvent, 10 μL of standard solution, and 10 μL of sample solution, respectively, and inject them into the liquid chromatograph for detection, and record the solvent chromatogram, standard chromatogram, and sample solution chromatogram respectively;

[0011] Purity calculation: Obtain the solvent peak from the solvent chromatogram, obtain the retention time of erythrose disulfate from the standard chromatogram, remove the solvent peak from the detection chromatogram, and calculate the ratio of the erythrose disulfate peak area in the sample solution chromatogram to the total area of all peaks to obtain the purity of erythrose disulfate.

[0012] On the basis of the above technical solution, the detector of the liquid chromatograph is a differential detector, and the detector temperature is 40°C.

[0013] On the basis of the above technical solution, a reverse phase chromatography column with octadecyl bonded silica gel as filler is used, with specifications of 250mm*5μm*4.6mm, such as Agilent 5HC-C18(2)250*4.6mm.

[0014] Based on the above technical solution, the preferred mobile phase is a mixed solution of methanol and pure water, a mixed solution of acetonitrile and pure water, and the most preferred is a mixed solution of acetonitrile and pure water, and the optimal volume ratio of acetonitrile in the mixed solution is 35%.

[0015] Based on the above technical solution, the optimal flow rate is 1 mL / min.

[0016] Based on the above technical solution, the optimal column temperature is 40°C.

[0017] On the basis of the above technical solution, acetonitrile is directly selected to dissolve the sample and then inject it.

[0018] Based on the above technical solution, the injection concentration can be ensured to be within the detection range of the equipment. Generally, the injection concentration is 1-10 mg / mL; in order to increase the exposure to impurities, the optimal concentration is 40 mg / mL.

[0019] The present invention uses a common high performance liquid chromatograph equipped with a differential detector, such as Shimadzu.

[0020] The HPLC-RID purity detection method of erythrose disulfate of the present invention has the following beneficial effects:

[0021] The invention provides an HPLC-RID purity detection method for erythrose disulfate, which adopts a liquid chromatograph for detection, has simple operation, high accuracy, good repeatability, and good application prospect. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0023] Figure 1 This is a liquid phase detection chromatogram of erythrose disulfate according to Example 1 of the present invention;

[0024] Figure 2 This is a liquid phase detection chromatogram of erythrose disulfate according to Example 2 of the present invention;

[0025] Figure 3This is a liquid phase detection chromatogram of erythrose disulfate according to Example 3 of the present invention. DETAILED DESCRIPTION

[0026] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts shall fall within the scope of protection of the present invention.

[0027] Example 1

[0028] Weigh 0.5 g of erythrose disulfate standard into a clean container, pipette 25 ml of acetonitrile to dissolve, to obtain a standard solution, set aside; then weigh 0.5 g of erythrose disulfate sample into a clean container, pipette 25 ml of acetonitrile to dissolve, to obtain a sample solution, set aside.

[0029] Weigh 10 μL of blank solvent, 10 μL of standard solution, and 10 μL of sample solution, respectively, and inject them into the liquid chromatograph for detection in sequence, and record the solvent chromatogram, standard chromatogram, and sample solution chromatogram respectively.

[0030] The sample was injected in parallel 6 times, and the retention time, peak area and purity of erythrose disulfate were recorded after detection.

[0031] The detector for HPLC was a differential detector, and the detector temperature was 40°C.

[0032] The chromatographic column filler is octadecyl bonded silica gel with a specification of 250mm*5μm*4.6mm.

[0033] The mobile phase in HPLC was a mixed solution of methanol and pure water, with the volume ratio of methanol in the mixed solution being 40%.

[0034] The flow rate in HPLC was 1 mL / min.

[0035] The column temperature in HPLC was 40°C.

[0036] Acetonitrile is used as a solvent, and a solvent peak is obtained by detection. The standard sample is detected and used to determine the retention time of erythrose disulfate. The detection spectrum of the sample solution is superimposed with the solvent peak to obtain a detection peak. The purity of erythrose disulfate can be calculated based on the integral of the detection peak and the integral of the peak area of erythrose disulfate. The calculation method is the peak area of erythrose disulfate divided by the sum of all peak areas * 100%.

[0037] The test results are shown in Table 1 below:

[0038] Table 1

[0039]

[0040]

[0041] The peak areas of the test results are shown in Table 2 below:

[0042] Table 2

[0043]

[0044] The purity test results are shown in Table 3 below:

[0045] Table 3

[0046]

[0047] From the above result data, it can be seen that the standard deviation of the purity determination of erythrose disulfate is 0.1802, and the relative standard deviation is 0.181%. It can be seen that the repeatability of this method is good and the accuracy is high.

[0048] Example 2

[0049] Except that the mobile phase in the detection conditions was changed to 35% acetonitrile aqueous solution, other steps and conditions were the same as those in Example 1.

[0050] The test results are shown in Table 4 below:

[0051] Table 4

[0052]

[0053]

[0054] The peak areas of the test results are shown in Table 5 below:

[0055] Table 5

[0056]

[0057] The purity test results are shown in Table 6 below:

[0058] Table 6

[0059]

[0060] From the above result data, it can be seen that the standard deviation of the purity determination of erythrose disulfate is 0.07583, and the relative standard deviation is 0.076%. It can be seen that the repeatability of this method is good and the accuracy is high.

[0061] Example 3

[0062] Except that the mobile phase in the detection conditions was changed to 35% acetonitrile aqueous solution and the sample solution was changed to 40 mg / mL, other steps and conditions were the same as those in Example 1.

[0063] The test results are shown in Table 7 below:

[0064] Table 7

[0065]

[0066]

[0067] The peak areas of the test results are shown in Table 8 below:

[0068] Table 8

[0069]

[0070] The purity test results are shown in Table 9 below:

[0071] Table 9

[0072]

[0073] From the above result data, it can be seen that the standard deviation of the purity determination of erythrose disulfate is 0.06006, and the relative standard deviation is 0.060%. It can be seen that the repeatability of this method is good and the accuracy is high.

[0074] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A HPLC-RID purity detection method for erythrose disulfate, characterized in that: The steps include: Prepare blank solvent: take appropriate amount of acetonitrile and set aside; Prepare standard solution: weigh erythrose disulfate standard into a clean container, pipette acetonitrile to dissolve, and obtain standard solution for later use; Prepare sample solution: weigh erythrose disulfate sample into a clean container, pipette acetonitrile to dissolve it to obtain standard solution, set aside; Sampling: Take blank solvent, standard solution and sample solution respectively, inject them into liquid chromatograph in sequence for detection, and record the solvent chromatogram, standard chromatogram and sample solution chromatogram respectively; Purity calculation: Obtain the solvent peak from the solvent chromatogram, obtain the retention time of erythrose disulfate from the standard chromatogram, remove the solvent peak from the detection chromatogram, and calculate the ratio of the erythrose disulfate peak area in the sample solution chromatogram to the total area of all peaks to obtain the purity of erythrose disulfate.

2. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The mass volume ratio of erythrose disulfate standard to acetonitrile was 0.04 g / mL.

3. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The mass volume ratio of erythrose disulfate sample to acetonitrile was 0.04 g / mL.

4. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The detector of the liquid chromatograph is a differential detector, and the detector temperature is 40°C.

5. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The reverse phase chromatography column using octadecyl bonded silica as filler has a specification of 250mm*5μm*4.6mm.

6. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The mobile phase was a mixture of methanol and pure water, or a mixture of acetonitrile and pure water.

7. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The mobile phase is a mixed solution of acetonitrile and pure water in a volume ratio of 35:

65.

8. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The flow rate was 1 mL / min.

9. The HPLC-RID purity detection method of erythrose disulfate as claimed in claim 1, wherein The column temperature of the reverse phase chromatography was 40 °C.

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