Method for separating and detecting folic acid and folic acid optical isomers in folic acid

A technology of optical isomers and folic acid, applied in the field of drug analysis, can solve the problems of difficult separation and drug analysis obstacles, and achieve the effect of simple method and fast peak time

Active Publication Date: 2021-04-13
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned substances are optical isomers of folic acid, which have similar properties and structures, and their separation is more difficult. At present, there is no relevant technical disclosure to separate them from many impurities, so the analysis of optical isomers of folic acid is still a difficult task. Technical problems, obstacles to the analysis of related drugs

Method used

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  • Method for separating and detecting folic acid and folic acid optical isomers in folic acid
  • Method for separating and detecting folic acid and folic acid optical isomers in folic acid
  • Method for separating and detecting folic acid and folic acid optical isomers in folic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Main instruments: Shimadzu LC-20A high performance liquid chromatography.

[0056] mobile phase:

[0057] Mobile phase A: methanol: 40-60, acetonitrile: 40-60;

[0058] Mobile phase B: acetic acid: 2-4, triethylamine: 2-4;

[0059] Methanol-acetonitrile-acetic acid-triethylamine (40~60:40~60:2~4:2~4), the best effect group is 50:50:3:3;

[0060] Chromatographic column: O-9-(tert-butylcarbamoyl)quinine covalently bonded to the surface of silica gel as filler, 4.6mm×150mm, 5μm;

[0061] Flow rate: 0.4~0.6ml / min;

[0062] Detection wavelength: 280±10nm;

[0063] Column temperature: 20-30°C, preferably 25°C;

[0064] Diluent: tetrahydrofuran - methanol - water - acetic acid - triethylamine (10:80:10:2.4:3);

[0065] Injection volume: 5μl;

[0066] The test solution: 0.3mg / ml;

[0067] Quantitative method: peak area normalization method.

Embodiment 2

[0069] Solution preparation:

[0070] Avoid light operation.

[0071] The test solution: take an appropriate amount of this product (folic acid), add diluent [tetrahydrofuran-methanol-water-acetic acid-triethylamine (10:80:10:2.4:3)] ultrasonically dissolve and quantitatively dilute to make 1ml Contain about 0.3mg of the solution, shake well, that is.

[0072] System suitability solution: Take an appropriate amount of folic acid optical isomer system suitability reference substance (containing folic acid and optical isomer), add diluent to ultrasonically dissolve and dilute to make a solution containing about 0.3mg per 1ml, shake well, that is have to.

Embodiment 3

[0074] testing method

[0075] Precisely measure 5 μl of the system suitability solution, inject it into the liquid chromatograph, and record the chromatogram. figure 1 ).

[0076] Table 1 Integral results of system suitability testing

[0077]

[0078] All impurities of folic acid are mixed, including impurities A, B, C, D, E, F, G, H and SM1d, SM1k and folic acid optical isomer impurities in EP standard (attached figure 2 ).

[0079] Other impurities in folic acid are mixed, including EP impurities A, B, C, D, E, F, G, H and SM1d, SM1k (attached image 3 ).

[0080] Precisely measure 5 μ l of the test solution, inject it into a liquid chromatograph, record the chromatogram to 2.5 times the retention time of the main peak, and calculate the content of the optical isomers by the peak area normalization method for the two peaks of the optical isomers and folic acid. The content of isomers does not exceed 0.15%.

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Abstract

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and detecting folic acid and optical isomers thereof. A chromatographic column adopted by the method takes silica gel surface covalent bonding O-9-(tert-butylcarbamoyl) quinine as a filler, an organic solvent, organic acid and triethylamine are adopted for gradient elution. the folic acid and / or the folic acid optical isomer are / or is separated; the flow velocity of the mobile phase is 0.4-0.6 ml / min; the column temperature of the chromatographic column is 20-30 DEG C; the wavelength of the detector is set to be 280 + / -10nm; the used diluent is a mixed solution of tetrahydrofuran, methanol, water, acetic acid and triethylamine, and the contents of folic acid and optical isomers thereof are measured by using a peak area normalization method. According to the method, the peak appearing time of the folic acid and the optical isomer thereof is short, the operation can be finished within 20 minutes, peak patterns are symmetrical, the folic acid and the optical isomer thereof can be separated from various impurities to obtain the accurate content, and the method is simple, quick and effective.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for separating and detecting folic acid and folic acid optical isomers in folic acid by HPLC. Background technique [0002] Folic acid is a water-soluble vitamin with the molecular formula C 19 h 19 N 7 o 6 , molecular weight 441.40, chemical name N-[4-[(2-amino-4-oxo-1,4-dihydro-6-pteridine)methylamino]benzoyl]-L-glutamic acid. It is named for its rich content in green leaves, also known as pteroyl glutamic acid. There are several forms of existence in nature, and its parent compound is composed of three components of pteridine, p-aminobenzoic acid and glutamic acid. Its structural formula is as follows: [0003] [0004] Folic acid is in the form of yellow or orange flakes or needle-like crystals, odorless and tasteless, when heated to about 250°C, the color gradually becomes darker, and finally turns into a black jelly. Not easily soluble in water and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/04G01N30/06G01N30/8634G01N2030/042
Inventor 周书荣李冰洁陈雯杜帅兰昌云刘阔
Owner CHONGQING HUABANGSHENGKAI PHARM
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