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Method for detecting related substances in sodium levofolinate raw material and preparation of sodium levofolinate raw material

A technology for sodium levofolinate and related substances, which is applied in measurement devices, material separation, and analysis of materials, etc., can solve the problems of blocking the expansion of thymidylate synthase and increasing the inhibitory effect of DNA biosynthesis, and achieves high sensitivity and exclusive use. The effect of sex, simple operation

Inactive Publication Date: 2020-07-14
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This increases the inhibition of DNA biosynthesis, leading to an extended block of thymidylate synthase

Method used

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  • Method for detecting related substances in sodium levofolinate raw material and preparation of sodium levofolinate raw material
  • Method for detecting related substances in sodium levofolinate raw material and preparation of sodium levofolinate raw material
  • Method for detecting related substances in sodium levofolinate raw material and preparation of sodium levofolinate raw material

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Experimental program
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Effect test

Embodiment 1

[0041] The choice of solvent and the choice of the concentration of need testing solution:

[0042] The choice of solvent for dissolving the sample, we dissolve the sample with water, acetonitrile, ethanol, and mobile phase respectively, among which water has the best solubility for the sample.

[0043]We use the mobile phase as the solvent of the sample, which are respectively formulated as 0.5mg / mL, 0.6mg / mL and 0.7mg / mL. 0.7mg / mL is more suitable for the detection of impurities in the sample. We finally choose 0.7mg / mL as the sample solvent. The concentration of the test solution.

Embodiment 2

[0045] Selection of salt solution in mobile phase:

[0046] Various salt solutions are commonly used in liquid chromatography, such as: disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, ammonium dihydrogen phosphate, diamine hydrogen phosphate, ammonium formate or acetic acid Amines etc. The ion pair reagent is selected from tetrabutylammonium hydroxide, cetyltrimethylammonium bromide, tetrabutylammonium bromide, sodium heptanesulfonate, sodium octanesulfonate, sodium hexanesulfonate or Sodium Dialkyl Sulfonate.

[0047] For the selection of the concentration of the salt solution, we have investigated the concentration of the salt solution, and determined that the concentration is 0.005-0.02mol / L as the appropriate concentration range, and the optimal concentration is 0.01mol / L.

Embodiment 3

[0049] 1) Instruments and testing conditions

[0050] Waters 1525 liquid chromatograph produced by Waters Corporation in the United States, automatic sampler, PDA detector, chromatographic column: ZORBAX Eclipse Plus C18 (5.0μm, 4.6×250mm); detection wavelength: 280mn; column temperature: 40°C; Use disodium hydrogen phosphate buffer solution (take 4 mL of 25% tetrabutylammonium hydroxide and 3.6 g of disodium hydrogen phosphate dodecahydrate, add 1000 mL of water to dissolve, stir for 10 min, adjust pH to 7.5 with 40% phosphoric acid) as phase A, and use methanol For phase B, perform linear gradient elution according to the following table:

[0051] time (minutes) Mobile phase A(%) Mobile phase B(%) 0 83 17 25 83 17 35 75 25 45 70 30 51 70 30 52 83 17 75 83 17

[0052] 2) Experimental steps 1. Preparation of solution:

[0053] Preparation of impurity stock solution: Take an appropriate amount of impurity reference su...

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Abstract

The invention provides a method for detecting related substances in a sodium levofolinate raw material and a preparation of the sodium levofolinate raw material, the method is carried out by adoptinga high performance liquid chromatography, and the chromatographic conditions are as follows: a chromatographic column is an octadecylsilane chemically bonded silica chromatographic column; the mobilephase A is a salt solution; the pH value of the salt solution is 6.0 to 9.0; the mobile phase B is a mixed solution of any one or two of acetonitrile, methanol and ethanol; the salt solution is a saltsolution containing an ion pair reagent; a gradient elution method is adopted, the flow velocity of a mobile phase is 0.2-1.2 ml / min, the column temperature of a chromatographic column is 35-45 DEG C, and the detection wavelength is 200-300 nm; the detection method is simple and convenient to operate, high in separation degree, high in specificity and accurate and credible in detection result.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a method for detecting related substances in sodium levofolinate raw materials and preparations thereof and an application thereof. Background technique [0002] Sodium levofolinate (English name: Disodium Levofolinate) chemical name is (2S)-2-[[4-[[[(6S)-2-amino-5-formyl-1,4,5,6,7, 8-Hexahydro-4-oxo-6-piperidinyl]methyl]amino]benzoyl]amino]-glutaric acid disodium salt, molecular formula C 20 h 21 Na 2 N 7 o 7 , molecular weight 517.40, CAS accession number: [0003] 284461-73-0. Its structure is shown in formula I. [0004] [0005] Levofolinic acid sodium was approved for marketing in the UK on March 19, 2008, and has been listed in more than 20 countries including Germany, France, and Belgium. The treatment can reduce the toxic and side effects of chemotherapy drugs and improve the quality of life of tumor patients, which has significant clinical s...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74G01N30/64G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/64G01N30/74G01N30/8634
Inventor 雷勇胜康江鹏魏巍潘毅
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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