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HPLC analysis of impurities in dianhydrogalactitol

A technology of dianhydrodulcitol and dulcitol, which is applied in the field of HPLC analysis of impurities in dianhydrodulcitol, and can solve the problem of high incidence

Active Publication Date: 2017-12-29
DEL MAR PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to their sensitivity to pollutants, these patients may experience a higher incidence of unwanted side effects

Method used

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  • HPLC analysis of impurities in dianhydrogalactitol
  • HPLC analysis of impurities in dianhydrogalactitol
  • HPLC analysis of impurities in dianhydrogalactitol

Examples

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Embodiment 1

[0083] Example 1. HPLC Analysis of Didehydrodulcitol Preparation Using Isocratic Sodium Hydroxide Elution

[0084] Dulcitol and related impurities in pharmaceutical formulations of didhydrodulcitol were determined by ion-exchange high performance liquid chromatography with differential refractive index detection using the procedure disclosed in this example.

[0085] During this process, the sample was prepared so that the target concentration of dianhydrodulcitol was 5 mg / mL. An anion exchange column (Hamilton RCX-10, 250*4.1 mm, 7 μm), 50 mM NaOH was used as the isocratic mobile phase, and differential refractive index detection were used to separate dulcitol, didhydrodulcitol, and related impurities. The concentration of dulcitol was determined using an external standard, and the amount of related substances was estimated using a DAG reference standard.

[0086] A suitable HPLC system and data acquisition system is an Agilent Technologies 1200 Series HPLC system or equival...

Embodiment 2

[0108] Example 2. HPLC Analysis with Evaporative Light Scattering Detector and Using Water / Acetonitrile Gradient

[0109] To improve the separation of impurities, another HPLC analysis method was employed in which an evaporative light scattering detector (ELSD) with a water / acetonitrile gradient as detailed below was used.

[0110] Due to the limitations of refractive index (RI) displays, HPLC / RI methods are not specific enough to obtain reliable impurity profile data, potentially creating an unacceptable risk of exposing patients to unknown or incompletely characterized impurities. To solve this problem, a more sensitive detector such as the Evaporative Light Scattering Detector (ELSD) manufactured by Agilent (Agilent) is used in conjunction with the HPLC system to detect the presence of Dicrol in bulk drug or finished drug. impurities found in.

[0111] For example, analyze a DAG sample by HPLC / ELSD method using a YMC C18 column and the gradient shown in Table 3:

[0112] ...

Embodiment 3

[0118] Example 3. HPLC analysis using an aqueous formic acid / methanol gradient to improve separation of monoepoxide peaks

[0119] To improve the separation of the monoepoxide peak, a new method was developed. This new method employed the following parameters: The column was Atlantis C18, 250 x 4.6 mm, 5 μm. The column temperature was 30°C. The flow rate was 0.5 mL / min. The injection volume was 100 μL. The ELSD detector was operated in cooling mode with a drift tube temperature of 35°C, a gain of 400, 2pps, and 45PSI. Mobile phase A was 0.05% formic acid in water. Mobile phase B was 100% methanol. Gradients are shown in Table 5:

[0120] table 5

[0121]

[0122]

[0123] Better separation of early eluting impurities has been observed (referred to as Figure 5 Chromatogram of the DAG sample below). Peak 2, labeled dulcitol, eluted at a retention time of 6.26 minutes or a relative retention time (RRT) of 0.59. The dianhydrodulcitol eluted at 10.86 minutes.

[0...

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Abstract

An improved analytical method for analysis of dianhydrogalactitol preparations provides a method for determining the purity of dianhydrogalactitol and detecting impurities in preparations of dianhydrogalactitol, as well as identifying any such impurities. The method employs high performance liquid chromatography (HPLC), in particular, HPLC with evaporative light scattering detection (ELSD); the HPLC can be followed by tandem mass spectroscopy. The method can further comprise the step of performing preparative HPLC collection of at least one specific substance peak present in a preparation of dianhydrogalactitol.

Description

[0001] cross reference [0002] This application claims the rights and interests of the US patent application titled "Improved Analytical Methods for Analyzing and Determining Impurities in Dianhydrogalactitol" filed by Xiaoyun Lu and Mike Li on November 18, 2013 and numbered US 14 / 083,135; US 14 / 083,135 claims Xiaoyun Lu's U.S. Patent Application Serial No. US13 / 933,844, filed July 2, 2013, entitled "Improved Analytical Methods for Analyzing and Determining Impurities in Dianhydrogalactitol," and is a continuation-in-part of the latter; US13 / 933,844 pursuant to Preface asserting interest in PCT application titled "Improved Analytical Methods for Analyzing and Determining Impurities in Dianhydrogalactitol" filed by Xiaoyun Lu on February 26, 2013, serial number PCT / IB2013 / 000793, and part of the latter designating the United States Consecutive case; PCT / IB2013 / 000793 sequentially claimed the rights and interests of Xiaoyun Lu’s U.S. provisional patent application titled “Improve...

Claims

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Application Information

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IPC IPC(8): C07D301/02C07D303/14G01N30/22G01N30/74
CPCC07D301/02C07D303/14G01N30/74G01N30/88G01N2030/8494G01N2030/8872C07D307/02G01N30/72
Inventor 刘晓云
Owner DEL MAR PHARMA
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