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Optical purity analysis method of pasireotide starting material

A technology of optical purity and pasireotide, which is applied in the field of optical purity analysis of pasireotide starting materials, can solve the problems of ineffective control of the optical purity of amino acids, no chromogenic groups in molecules, large method errors, etc. Fast, high sensitivity, fast and accurate analysis, convenient effect

Active Publication Date: 2020-06-23
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, due to the simple molecular structure and small molecular weight of N(e)-tert-butoxycarbonyl lysine, and the molecule itself has no chromophore, it has no absorption and / or terminal absorption is very weak under ultraviolet light, under ordinary chromatographic conditions No response, difficult to detect directly by ordinary liquid chromatography
In the traditional method, the method of measuring the specific rotation is mainly used to control the optical purity of amino acids and their derivatives. However, due to the limitations of specificity and sensitivity, the method has large errors, poor repeatability, and cumbersome operation. The specific rotation method cannot effectively control Optical purity of amino acids, especially for protected amino acids with small specific rotation values

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  • Optical purity analysis method of pasireotide starting material
  • Optical purity analysis method of pasireotide starting material
  • Optical purity analysis method of pasireotide starting material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0120] The optical purity test method of N(e)-tert-butoxycarbonyllysine:

[0121] Chromatographic column: ChiralPak ZWIX(+), 4×150 nm, 3 μm.

[0122] Mobile phase: A: methanol; B: acetonitrile; methanol: acetonitrile (40:60) + 50mM formic acid + 25mM diethylamine;

[0123] Flow rate: 0.4mL / min;

[0124] Column temperature: 25°C;

[0125] Elution method: isocratic elution;

[0126] Detection wavelength: 220nm;

[0127] Injection volume: 10 μL.

[0128] Preparation of the control sample solution: Accurately weigh appropriate amounts of (S)-type N(e)-tert-butoxycarbonyllysine and (R)-type N(e)-tert-butoxycarbonyllysine standard substances respectively, add ACN: H 2 O(1:1)+1%TFA dissolved and diluted to make about 10mg of S-type N(e)-tert-butoxycarbonyllysine and R-type N(e)-tert-butoxycarbonyllysine per 1mL Amino acid was passed through a 0.45 μm microporous membrane as a reference solution.

[0129] Configuration of the test sample solution: Accurately weigh an appropria...

Embodiment 2

[0134] The optical purity test method of N(e)-tert-butoxycarbonyllysine:

[0135] Chromatographic column: ChiralPak ZWIX(+), 250×4 nm, 3 μm.

[0136] Mobile phase: A: methanol; B: acetonitrile; methanol: acetonitrile (40:60) + 50mM acetic acid + 25mM triethylamine solution;

[0137] Flow rate: 0.6mL / min;

[0138] Column temperature: 30°C;

[0139] Elution method: isocratic elution;

[0140] Detection wavelength: 220nm;

[0141] Injection volume: 10 μL.

[0142] Preparation of the control sample solution: Accurately weigh appropriate amounts of (S)-type N(e)-tert-butoxycarbonyllysine and (R)-type N(e)-tert-butoxycarbonyllysine standard substances respectively, add ACN: H 2 O(1:1)+1%TFA dissolved and diluted to make about 20mg of (S)-type N(e)-tert-butoxycarbonyllysine and R-type N(e)-tert-butoxylysine per 1mL Carbonyl lysine was passed through a 0.45 μm microporous membrane as a reference solution.

[0143] Configuration of the test sample solution: Accurately weigh an ...

Embodiment 3

[0148] The optical purity test method of N(e)-tert-butoxycarbonyllysine:

[0149] Chromatographic column: ChiralPak ZWIX(+), 200×4.6 nm, 3 μm.

[0150] Mobile phase: A: methanol; B: acetonitrile; methanol: acetonitrile (40:60) + 50mM propionic acid + 25mM ammonia solution;

[0151] Flow rate: 0.2mL / min;

[0152] Column temperature: 20°C;

[0153] Elution method: isocratic elution;

[0154] Detection wavelength: 220nm;

[0155] Injection volume: 10 μL.

[0156] Preparation of the control sample solution: Accurately weigh appropriate amounts of (S)-type N(e)-tert-butoxycarbonyllysine and (R)-type N(e)-tert-butoxycarbonyllysine standard substances respectively, add ACN: H 2 O(1:1)+1%TFA dissolved and diluted to make about 15mg (S)-type N(e)-tert-butoxycarbonyllysine and R-type N(e)-tert-butoxylysine per 1mL Carbonyl lysine was passed through a 0.45 μm microporous membrane as a reference solution.

[0157] Configuration of the test sample solution: Accurately weigh an appr...

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Abstract

The invention provides an optical purity analysis method of a pasireotide starting material. The method comprises the following steps: respectively preparing a test solution and a reference solution;according to preset chromatographic conditions, on the basis of a chiral chromatographic column, the test solution and the reference solution being subjected to sample introduction and elution throughHPLC; respectively recording chromatograms of the test solution and the reference solution; and based on an area normalization method, calculating the optical purity of (S)-type N (e)-tert-butyloxycarboryl lysine according to the chromatogram and the peak area. The optical purity analysis method provided by the invention is high in sensitivity, the accuracy of chiral analysis of the (S)-type N (e)-tert-butyloxycarbonyl lysine compound is improved, the reproducibility is good, the operation method is simple, the speed is high, the efficiency is high, and convenience is provided for rapid and accurate analysis of the optical purity of (S)-type N (e)-tert-butyloxycarbonyl lysine.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to an optical purity analysis method of a pasireotide starting material. Background technique [0002] Pasireotide is a multi-receptor targeting somatostatin (SST) inhibitor analogue that can bind to 4 of the 5 somatostatin receptor (SST Receptor, SSTR) subtypes with high affinity (SST1 ,2,3,5), exert its pharmacological effects by binding to somatostatin receptors. It is a peptide drug developed by Novartis Pharma AG of Switzerland. It was first approved for marketing by the EU drug regulatory authority in accordance with the relevant regulations on rare diseases on April 25, 2012. The trade name is Signifor, and it was released on December 14, 2012. It has been approved by the US FDA for the treatment of adrenal hyperactivity and Cushing's disease that cannot be treated by surgery, and has been approved for marketing in 48 countries. [0003] [0004] N(e)-tert-butoxycarb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/64
CPCG01N30/02G01N30/64Y02P20/55
Inventor 吴砺高红旗李孝吴醇李雷
Owner WUHAN WUYAO SCI & TECH