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HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester

A technology of thiamphenylphenylserine ethyl ester and content, which is applied in the field of pharmaceutical and chemical quality inspection, and achieves the effects of good specificity, good reproducibility, and simple method

Active Publication Date: 2010-09-15
HUBEI LONGXIANG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, only the routine physical and chemical indicators of D-p-thiamphenyl phenylserine ethyl ester are usually detected, and in the production process, a small amount of L-p-thiamphene Phenylserine ethyl ester is difficult to truly reflect its quality status only by conventional physical and chemical indicators, so establishing a method that can accurately measure the content of D-p-thymphenyl phenylserine ethyl ester will have great guiding significance for its production, and more Can reduce the cost and improve the quality of Florfenicol

Method used

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  • HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester
  • HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester
  • HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Chiral column with cellulose-tris(4-methylbenzoate) stationary phase coated on silica gel surface, column length 150mm×inner diameter 4.6mm×filler particle size 5μm, mobile phase is n-hexane: acetonitrile: ethylenediamine =40:60:0.1, the flow rate is 0.4ml / min, the detection wavelength is 210nm, the column temperature is 32°C, and the injection volume is 5μL. Accurately weigh 25 mg of D-p-methylsulfonyl phenylserine ethyl ester sample (batch: 090501) into a 25 ml volumetric flask, add an appropriate amount of n-propanol: methanol (1:1, v / v) solvent to dissolve it by ultrasound, and then Add the above-mentioned mixed solvent of n-propanol and methanol to dilute to the mark, and filter with 0.22μm filter membrane before sample injection for chromatographic analysis.

[0028] Take the above-mentioned solution to be tested, inject it into the chromatograph, measure twice in parallel, record the detection time for 40 minutes, obtain the chromatogram, calculate the content of D-...

Embodiment 2

[0030] Chiral column with cellulose-tris(4-methylbenzoate) stationary phase coated on silica gel surface, column length 150mm×inner diameter 4.6mm×filler particle size 10μm, mobile phase is n-hexane: methanol: ethylenediamine =60:40:0.8, the flow rate is 1.5ml / min, the detection wavelength is 235nm, the column temperature is 39°C, and the injection volume is 20μL. Accurately weigh 25 mg of D-p-methylsulfonyl phenylserine ethyl ester sample (batch: 090502) into a 25ml volumetric flask, add an appropriate amount of n-propanol: methanol (1:1, v / v) solvent to dissolve it by ultrasound, and then Add the above-mentioned mixed solvent of n-propanol and methanol to dilute to the mark, filter with 0.45μm filter membrane before sample injection, for chromatographic analysis.

[0031] Take the above-mentioned solution to be tested, inject it into the chromatograph, measure twice in parallel, record the detection time for 40 minutes, obtain the chromatogram, calculate the content of D-p-meth...

Embodiment 3

[0033] A chiral column with cellulose-tris(4-methylbenzoate) stationary phase coated on silica gel surface, column length 250mm×inner diameter 4.6mm×filler particle size 5μm, mobile phase is n-hexane: absolute ethanol: two Ethylamine=60:40:0.5, the flow rate is 1.2ml / min, the detection wavelength is 220nm, the column temperature is 35°C, and the injection volume is 20μL. Accurately weigh 25mg of D-p-methylsulfonylphenylserine ethyl ester sample (batch: 090503) into a 25ml volumetric flask, add an appropriate amount of n-propanol: methanol (1:1, v / v) solvent to dissolve it by ultrasound, and then Add the above-mentioned mixed solvent of n-propanol and methanol to dilute to the mark, filter with 0.45μm filter membrane before sample injection, for chromatographic analysis.

[0034] Take the above-mentioned solution to be tested, inject it into the chromatograph, measure twice in parallel, record the detection time for 40 minutes, obtain the chromatogram, calculate the content of D-p...

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Abstract

The invention discloses an HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester, comprising the following steps of: preparing a solution from D-4-methylsulfonylphenyl serine ethyl ester with a mixed solvent of normal propyl alcohol and carbinol; filtering with a microporous membrane; coating the chiral column of the stationary phase of cellulose-tris (4-methyl benzoate) on the surface of silica gel; detecting in the presence of proper detection wavelength, flow rate and column temperature by taking a mixed solution of normal hexane, an organic modifier and organic base; and then calculating the content of a sample according to a spectrogram. The D-4-methylsulfonylphenyl serine ethyl ester and L-4-methylsulfonylphenyl serine ethyl ester can be effectively separated, and the content of the D-4-methylsulfonylphenyl serine ethyl ester can be accurately measured by adopting the method. The method is simple and convenient, reliable and rapid and has high sensitivity and good repeatability and specificity and lays foundation for the formulation of the quality standard of the D-4-methylsulfonylphenyl serine ethyl ester.

Description

Technical field [0001] The invention relates to an HPLC (High Performance Liquid Chromatography) method for determining the content of D-p-methylsulfonyl phenylserine ethyl ester, and belongs to the field of pharmaceutical and chemical quality detection. Background technique [0002] D-p-methylsulfonyl phenylserine ethyl ester (C 12 H 17 NO 5 S) is the key starting material for the synthesis of antibacterial drugs florfenicol and thiamphenicol. Its chemical structure is: The quality of D-p-methylsulfonylphenylserine ethyl ester directly affects the yield and quality of florfenicol and thiamphenicol. Florfenicol is a product developed by Schering-Plough of the United States in the late 1970s. Its antibacterial activity against sensitive bacteria is similar to that of chloramphenicol and thiamphenicol, but it is still resistant to bacteria resistant to chloramphenicol and thiamphenicol. Sensitive, such as Escherichia coli, Klebsiella, Pasteurella hemolyticus, Staphylococcus aureus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/36
Inventor 王铭宏吴东林
Owner HUBEI LONGXIANG PHARMA TECH CO LTD
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