Method for measuring content of Meldrum's acid

A determination method and technology of Michaelis acid, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of unpublished high-performance liquid chromatography to determine the content of Michaelis acid, which cannot directly reflect the content of Michaelis acid, and cannot be used for quantitative analysis, etc. problem, to achieve the effect of large detection range, high accuracy and improved accuracy

Inactive Publication Date: 2019-11-12
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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AI Technical Summary

Problems solved by technology

Mel Christopher introduced the thin-layer chromatography method in the literature, but thin-layer chromatography can only be used for semi-quantitative analysis and cannot be used for accurate quantitative analysis
The websites of Sigma Aldrich and Alfa Aisha show that the acid-base titration method is used to detect its content, but the actual detection is the content of the product after Michaelis acid hydrolysis. This method cannot directly reflect the content of Michaelis acid, and before titration Sodium hydroxide titration solution and hydrochloric acid titration solution need to be configured, which is cumbersome and has large titration errors
[0005] There is no method disclosed in the prior art for the determination of Michaelis acid content by high performance liquid chromatography

Method used

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  • Method for measuring content of Meldrum's acid
  • Method for measuring content of Meldrum's acid
  • Method for measuring content of Meldrum's acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Accurately weigh 10 mg of the standard substance, place it in a 100 mL volumetric flask, add water to dissolve, dilute to the mark with water, and shake well. Draw 1.5mL with a syringe, then filter it with a 0.45μm organic filter head and transfer it to a 1.5mL sampling bottle to obtain a standard solution; accurately weigh 10mg of Michaelis acid sample, place it in a 100mL volumetric flask, add water to dissolve, and then Dilute to the mark with water and shake well. Draw 1.5mL with a syringe, then filter it with a 0.45μm organic filter head and transfer it to a 1.5mL injection bottle to obtain the test solution.

[0050] Chromatographic conditions: Agilent Agilent1260Infinity high performance liquid chromatography, YMC-Triart C18 (4.6mm × 250mm, 5 μm); mobile phase: methanol-0.05mol / L potassium dihydrogen phosphate buffered saline solution (adjust pH=7.0 with triethylamine) = 10:90 (V / V) mixed solution; detection wavelength 259nm; flow rate 1.0mL / min; column temperat...

Embodiment 2

[0063] Sample and standard preparation are the same as example 1

[0064] Chromatographic conditions: Agilent1 260Infinity HPLC, Venusil C18 Plus column (4.6×200mm, 5μm, 120A); mobile phase: methanol-potassium dihydrogen phosphate buffered saline solution (0.02mol / L potassium dihydrogen phosphate solution, with three Ethylamine adjusted pH = 7.0) = 30:70 (V / V) mixed solution; detection wavelength 257nm; flow rate 1.5mL / min; column temperature 35°C; acquisition time 20min.

[0065] According to the above-mentioned chromatographic conditions, the continuous sample injection of the standard product is 6 times, and its average peak area measured is 8090, and the RSD is 0.12%; the peak area of ​​the test product is 7951, and the Michaelis acid test product content is 98.28%.

Embodiment 3

[0067] Sample and standard preparation are the same as example 1

[0068] Chromatographic conditions: Agilent1 260Infinity HPLC, HypersilODS-2 column (150×4.6mm, 5μm); mobile phase: methanol-potassium dihydrogen phosphate buffered saline solution (0.03mol / L potassium dihydrogen phosphate solution, with triethyl Amine adjusted pH = 7.0) = 20:80 (V / V) mixed solution; detection wavelength 258nm; flow rate 0.8mL / min; column temperature 30°C; acquisition time 20min.

[0069] According to the above-mentioned chromatographic conditions, the continuous sample injection of the standard product is 6 times, and its average peak area measured is 8120, and the RSD is 0.15%; 98.30%.

[0070] The data of Examples 1-3 show that each sample can be completed within 20 minutes of running time, indicating that the detection speed is fast; each dosage is about 10 mg, and the injection volume is 10 μL, and the sample dosage is small, which can greatly save the sample dosage; its peak The RSD of t...

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Abstract

The invention discloses a method for measuring the content of Meldrum's acid and is characterized in that peak areas of Meldrum's acid in a solution of a Meldrum's acid standard product and a solutionof a Meldrum's acid sample for test are separately measured by high performance liquid chromatography; and according to the obtained peak areas, calculating the mass content of Meldrum's acid in thesolution of the Meldrum's acid sample for test by using an external standard method. The method, which specifically limits chromatographic conditions for applying high performance liquid chromatography to measure the content of Meldrum's acid, is a simple content detection method with good separation effect, high accuracy and high precision. The method has a wide detection range and is accurate indetection results.

Description

technical field [0001] The invention relates to a method for measuring Michaelis acid content, belonging to the technical field of organic content detection. Background technique [0002] Meldrum's acid, English name: Meldrum's acid, CAS number is 2033-24-1, molecular formula is C 6 h 8 o 4 , the molecular weight is 144.125, the melting point is 94°C, and the structural formula is as follows: [0003] [0004] Michaelis acid is an important intermediate in organic synthesis, which can be used in the synthesis of heterocyclic compounds, natural products, medicines and pesticides. It can undergo various types of reactions such as electrophilic substitution, nucleophilic substitution, and addition rearrangement under mild conditions, so it has high application value. At present, there are few studies on its content detection methods at home and abroad. Mel Christopher introduced the method of thin-layer chromatography in the literature, but thin-layer chromatography can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 刘云英徐久振
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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