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A method for analyzing d(-) p-hydroxyphenylglycine content in d(-) p-hydroxyphenylglycine methyl ester

A technology of p-hydroxyphenylglycine methyl ester and p-hydroxyphenylglycine, which is applied in the field of pharmaceutical, chemical, and pharmaceutical testing, can solve problems such as affecting yield and quality, poor precision, and undetermined analysis methods, and achieves high sensitivity and accurate results. , good reproducibility

Active Publication Date: 2021-08-03
SHANDONG HANXING PHARM TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But wherein D(-) p-hydroxyphenylglycine will directly affect its yield and quality
[0003] In the patent CN201310725200.9, it is mentioned that D(-) p-hydroxyphenylglycine esters are used as raw materials to synthesize β-lactone amide antibiotic enzymes. This synthesis method has defects such as difficulty in product filtration. Due to the presence of a small amount of L-p-hydroxybenzene in the raw materials Caused by glycine esters and unreacted D(-)-hydroxyphenylglycine, which was discussed for isomers, but did not study the residue of D(-)-hydroxyphenylglycine
[0004] In the CN201210196387.3 patent, it is mentioned that TLC is used to control the residue of D(-) p-hydroxyphenylglycine in the product, and the content of D(-) p-hydroxyphenylglycine methyl ester is analyzed by HPLC, but there is no D(-) in the finished product. The residue of hydroxyphenylglycine is controlled, and TLC is used to control the residue with poor precision and cannot be accurately quantitatively analyzed
[0005] At present, there is no detailed elaboration on the determination and analysis method of D(-) p-hydroxyphenylglycine content in D(-) p-hydroxyphenylglycine methyl ester

Method used

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  • A method for analyzing d(-) p-hydroxyphenylglycine content in d(-) p-hydroxyphenylglycine methyl ester
  • A method for analyzing d(-) p-hydroxyphenylglycine content in d(-) p-hydroxyphenylglycine methyl ester
  • A method for analyzing d(-) p-hydroxyphenylglycine content in d(-) p-hydroxyphenylglycine methyl ester

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Experimental program
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Effect test

Embodiment 1

[0045] Under selected chromatographic conditions: variable wavelength ultraviolet detector, detection wavelength: 226nm; flow rate: 1.5ml / min; column temperature: 25°C; injection volume: 5μl; chromatographic column: Ultimate XB-Phenyl(II);

[0046] Buffered saline solution: 10mM potassium dihydrogen phosphate + 10mM triethylamine hydrochloride (solvent is water), adjust pH to 3.5 with phosphoric acid.

[0047] Mobile phase A: buffered saline solution: acetonitrile = 98:2, mobile phase B: buffered saline solution: acetonitrile = 80:20. Elute with gradient ratios. The gradient elution program is shown in the table below:

[0048] time (min) 0 3 15 17 Mobile phase A, % 100 100 0 0 Mobile phase B, % 0 0 100 100

[0049] D(-)p-Hydroxyphenylglycine stock solution: Weigh 50 mg of D(-)p-Hydroxyphenylglycine reference substance into a 100ml volumetric flask, add 0.1% phosphoric acid to dissolve to volume, and shake well.

[0050]System suitability...

Embodiment 2

[0054] Under selected chromatographic conditions: variable wavelength ultraviolet detector, detection wavelength: 226nm; flow rate: 1.5ml / min; column temperature: 25°C; injection volume: 5μl; chromatographic column: Ultimate XB-Phenyl(II);

[0055] Buffered saline solution: 10mM potassium dihydrogen phosphate + 10mM triethylamine hydrochloride, adjust the pH to 3.5±0.2 with phosphoric acid.

[0056] The mobile phase is mobile phase A: buffered saline solution: acetonitrile = 98:2, mobile phase B: buffered saline solution: acetonitrile = 80:20. Elute with gradient ratio, add 1 needle of system adaptability solution, p-hydroxyphenylglycine / p-hydroxyphenylglycine methyl ester tailing factor ≤ 2.0, resolution of p-hydroxyphenylglycine and the nearest peak is not less than 1.5; enter the spiked sample For 2 injections of the solution, the absolute difference of the test results of the spiked sample solution requires p-hydroxyphenylglycine ≤ 0.1%, and the largest single unknown impu...

Embodiment 3

[0064] Under selected chromatographic conditions: variable wavelength ultraviolet detector, detection wavelength: 226nm; flow rate: change the flow rate to 1.4ml / min and 1.6ml / min. Column temperature: 25°C; Injection volume: 5μl; Chromatographic column: Ultimate XB-Phenyl(II);

[0065] Buffered saline solution: 10mM potassium dihydrogen phosphate + 10mM triethylamine hydrochloride, adjust the pH to 3.5 with phosphoric acid.

[0066] The mobile phase is mobile phase A: buffered saline solution: acetonitrile = 98:2, mobile phase B: buffered saline solution: acetonitrile = 80:20. Inject 1 injection of system adaptability solution, D(-) p-hydroxyphenylglycine / D(-) p-hydroxyphenylglycine methyl ester tailing factor ≤ 2.0, and the resolution of D(-) p-hydroxyphenylglycine and the nearest peak is not less than 1.5, 2 injections of the sample spiked solution; the absolute difference of the detection results of the spiked test solution requires D(-) p-hydroxyphenylglycine ≤ 0.1%, the ...

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Abstract

The invention discloses an HPLC method for determining the content of D(-)p-hydroxyphenylglycine in D(-)p-hydroxyphenylglycine methyl ester. The method is to prepare a solution of D(‑) p-hydroxyphenylglycine methyl ester with dilute acid solution, adopt a chemically bonded stationary phase chromatographic column, add organic base with buffer salt, and adjust pH to 0.8-12 with acid as buffer salt solution, buffered salt solution and organic phase modifier in an appropriate ratio for gradient elution, and then detect at an appropriate detection wavelength, flow rate and column temperature, and then calculate the sample content based on the spectrum. The method of the invention can effectively separate D(-)p-hydroxyphenylglycine methyl ester and D(-)p-hydroxyphenylglycine, and accurately measure the content of D(-)p-hydroxyphenylglycine. The method is simple, reliable and rapid , high sensitivity, good reproducibility and specificity, which established the foundation for the establishment of quality standards for D(‑) p-hydroxyphenylglycine methyl ester.

Description

technical field [0001] The invention relates to a method for measuring and analyzing D(-)p-hydroxyphenylglycine content in D(-)p-hydroxyphenylglycine methyl ester, which belongs to the field of medicine, chemical and pharmaceutical testing. Background technique [0002] D(-)p-Hydroxyphenylglycine methyl ester is an organic intermediate synthesis, prepared from D(-)p-Hydroxyphenylglycine and methanol, which can be used to synthesize amoxicillin, and the antibacterial activity of amoxicillin against sensitive bacteria Similar to chloramphenicol and thiamphenicol, but still susceptible to chloramphenicol and thiamphenicol-resistant bacteria, such as Escherichia coli, Klebsiella, Pasteurella hemolyticus, Staphylococcus aureus, pleuropneumonia Actinobacillus and Salmonella typhi, etc. However, D(-) p-hydroxyphenylglycine will directly affect its yield and quality. [0003] In the patent CN201310725200.9, it is mentioned that D(-) p-hydroxyphenylglycine esters are used as raw ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 虞相华武强段丽艳姜磊吴言琴赵惠娣
Owner SHANDONG HANXING PHARM TECH CO LTD
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