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Detection method for content of D-methyl p-hydroxyphenylglycinate

A technology of p-hydroxyphenylglycine methyl ester and a detection method, which is applied in the field of D-p-hydroxyphenylglycine methyl ester content detection, can solve the problem of no D-p-hydroxyphenylglycine methyl ester and the like, achieves time saving, simple operation, and improved performance. The effect of accuracy

Pending Publication Date: 2020-12-25
HENAN NEWLAND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the continuous improvement of national economic conditions, the quality requirements for D-p-hydroxyphenylglycine methyl ester in the market are also getting higher and higher. At present, there are several detection methods for the content of D-p-hydroxyphenylglycine methyl ester in the market, such as high Chloric acid titration, HPLC, etc., but there is no detailed description of the content analysis method of D-hydroxyphenylglycine methyl ester

Method used

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  • Detection method for content of D-methyl p-hydroxyphenylglycinate
  • Detection method for content of D-methyl p-hydroxyphenylglycinate
  • Detection method for content of D-methyl p-hydroxyphenylglycinate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1: The condition that HPLC method measures D-p-hydroxyphenylglycine methyl ester content is

[0054] Chromatographic column: C18 (4.6mm×250mm, 5μm); detection wavelength: 225nm; flow rate: 1.0mL / min; column temperature: 25°C, injection volume: 20μL. Preparation of D-p-hydroxyphenylglycine methyl ester mobile phase: Accurately weigh 13.61g of potassium dihydrogen phosphate, add 2000ml of water to dissolve, adjust PH=5.00 with sodium hydroxide solution, measure 123ml of acetonitrile and mix. Preparation of reference substance solution: Accurately weigh 20 mg of D-p-hydroxyphenylglycine methyl ester reference substance, put it in a 100ml volumetric flask, add mobile phase to dissolve and set the volume to the mark, and shake well. Preparation of sample solution: Accurately weigh 20mg of D-p-hydroxyphenylglycine methyl ester sample, put it in a 100mL volumetric flask, add mobile phase to dissolve and dilute to the mark, and shake well.

Embodiment 2

[0055] Embodiment 2: HPLC method measures the concrete determination of D-p-hydroxyphenylglycine methyl ester content

[0056]Chromatographic conditions: chromatographic column; C18 (4.6mm×250mm, 5μm) Dalian Yili special product; detection wavelength: 225nm; flow rate 1.0mL / min; column temperature: 25°, injection volume: 20μL. Sample injection: Draw 20 μL of D-p-hydroxyphenylglycine methyl ester reference substance and sample solution with a sample needle, and inject samples through a manual injector. Other peaks and D-hydroxyphenylglycine methyl ester peak separation should not be less than 1.5. Weigh respectively 20.08mg and 20.00mg of D-p-hydroxyphenylglycine methyl ester reference substance, dissolve and dilute to 100ml volumetric flask with mobile phase, carry out separation and detection by liquid chromatography according to the prescribed method, and obtain two corresponding peak areas of 8205.36035 , 8117.80029. Weigh two samples of D-p-hydroxyphenylglycine methyl es...

Embodiment 3

[0066] Embodiment 3: Determination of D-p-hydroxyphenylglycine methyl ester sample content precision

[0067] Measure with the method of embodiment 2, take three samples and carry out 2 measurements respectively. The results are as follows:

[0068] Precision Test Results

[0069]

[0070] For 3 D-p-hydroxyphenylglycine methyl ester samples, the content precision was determined, and the relative standard deviation (RSD) was ≤ 2.0%, which met the detection requirements.

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Abstract

The invention discloses a detection method for the content of D-methyl p-hydroxyphenylglycinate. According to the method, HPLC is adopted for measuring the content of D-methyl p-hydroxyphenylglycinate. D-methyl p-hydroxyphenylglycinate is dissolved with a prepared D-methyl p-hydroxyphenylglycinate diluent, the volume is fixed, D-methyl p-hydroxyphenylglycinate is eluted at different flow speeds through a C18 chromatographic column at a certain column temperature, detection is conducted through an ultraviolet detector, and the content of D-methyl p-hydroxyphenylglycinate is calculated accordingto an obtained spectrum. In order to prove that the analysis method has the advantages of being high in sensitivity, good in reproducibility, short in consumed time, high in result accuracy and the like, the analysis method is compared with a perchloric acid titration method in an experiment, and an experiment result proves that the content of D-methyl p-hydroxyphenylglycinate can be rapidly andaccurately measured by adopting the experiment method. The method plays a crucial role in measuring the content of D-methyl p-hydroxyphenylglycinate in the current market.

Description

technical field [0001] The invention belongs to the detection field of medicine, chemical industry and pharmacy, and particularly relates to a method for detecting the content of D-p-hydroxyphenylglycine methyl ester. Background technique [0002] D-hydroxyphenylglycine methyl ester (MethylD-(-)-4-hydroxy-phenylglycinate), the molecular formula is C 9 h 11 NO 3 , with a molecular weight of 181.19, which is a white or off-white crystalline powder with poor solubility in water. D-p-Hydroxyphenylglycine methyl ester is an important pharmaceutical intermediate, which is widely used at home and abroad, and can be used in the preparation of β-lactam antibiotics such as amoxicillin and axazole cephalosporin. It can be used in the synthesis of peptide hormones and pesticides. Such antibiotics have the advantages of strong bactericidal activity, low toxicity, wide indications and good clinical curative effect. With the continuous improvement of national economic conditions, the q...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/045
Inventor 谢建中张芦苇杨喜歌王利英张丽娟刘超师红亮
Owner HENAN NEWLAND PHARMA
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