Method for separating and determining posaconazole Z2 and impurities thereof

A technology for posaconazole and impurities, which is applied in the field of analytical chemistry, can solve problems such as insufficient precision, undisclosed methods for qualitative and quantitative analysis of posaconazole by liquid chromatography-mass spectrometry, and achieve the effect of improving the recovery rate

Active Publication Date: 2021-11-19
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses the liquid chromatography external standard method to detect and calculate the impurity content, and the accuracy is not high enough
[0005] Moreover, the prior art does...

Method used

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  • Method for separating and determining posaconazole Z2 and impurities thereof
  • Method for separating and determining posaconazole Z2 and impurities thereof
  • Method for separating and determining posaconazole Z2 and impurities thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] Embodiment 1 blank diluent verification

[0095] Use blank solvent to mix with impurity SM respectively 1l , SM 1k ,Z 2d and Z 2h Enter the liquid chromatography for analysis, and the analysis results are as follows: Figure 5-Figure 8 As shown, the blank solvent is in SM 1l , SM 1k ,Z 2d and Z 2h There is no chromatographic peak at the peak retention time, and there is no interference to the detection of impurities.

Embodiment 2

[0096] Example 2 Repeatability Verification of Reference Substance Solution

[0097] Prepare SM 1l , SM 1k ,Z 2d and Z 2h The reference substance solution, and accurately measure 20 μ l into the high-performance liquid chromatography-mass spectrometer, each impurity was injected 6 times, and the chromatographic data are shown in Table 3 below, wherein the chromatogram of the sixth injection of each impurity Such as Figure 9-Figure 12 Shown, as can be seen from Table 3, the reference substance solution injection repeatability is good.

[0098] Table 3 Impurity reference substance solution chromatogram situation

[0099]

[0100]

Embodiment 3

[0101] Example 3 Quantitative Limit Verification

[0102] For impurities SM 1k , SM 1l ,Z 2d and Z 2h Carry out quantitative limit test, test result is as shown in table 4 below, and its chromatogram is as follows Figure 13-15 As can be seen from the table, SM 1k , SM 1l ,Z 2d and Z 2h The quantitation limit concentrations are about 0.710ng / ml, 0.698ng / ml, 0.747ng / ml and 0.727ng / ml respectively, the quantitation limits are about 0.710ppm, 0.698ppm, 0.747ppm and 0.727ppm respectively, and the RSDs of the peak areas are all less than 15%, and the signal-to-noise ratio is greater than 10.

[0103] The limit of quantitation detection situation of table 4 impurity

[0104]

[0105]

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for separating and determining posaconazole Z2 and impurities thereof. The method comprises the following steps: carrying out gradient elution separation by using liquid chromatography, wherein a mobile phase of the liquid chromatography is a mixed solution of a mobile phase A and a mobile phase B, the mobile phase A is an ammonium acetate-formic acid-aqueous solution, and the mobile phase B is an organic solvent; and performing mass spectrometry detection by using a quadrupole mass spectrometer to realize quantitative analysis. According to the method, the detection limit reaches the extremely low concentration of 0.35 ng/ml, the control requirement of ICH can be met, the impurity limit needs to be controlled to be 2.5 ppm or below, Z2 and Z2h can be well separated, and the recovery rate of Z2h is increased to the qualified level.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for separating and measuring posaconazole Z 2 and its impurity methods. Background technique [0002] Posaconazole (posaconazole) is a derivative of itraconazole, suitable for fungemia caused by fungi of the genus Candida and Cryptococcus, respiratory, gastrointestinal, urinary tract mycosis, peritonitis, meningitis, etc. During the preparation of posaconazole API, the qualitative and quantitative analysis of impurities has a significant impact on the quality control of the API. However, the existing methods for qualitative and quantitative detection of posaconazole and its impurities either have a single impurity, or the accuracy of quantitative analysis is not high, so the detection limit is high and the sensitivity is low. [0003] Patent CN201810992890.7 discloses a posaconazole impurity detection method, which includes 1) dissolving different impuriti...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/34G01N30/88G01N30/86G01N30/04
CPCG01N30/02G01N30/72G01N30/34G01N30/88G01N30/8634G01N30/8679G01N30/04G01N2030/884G01N2030/8872G01N2030/047Y02P20/55
Inventor 薛倩颜波倪科刘靖榆周维张颖李力
Owner CHONGQING HUAPONT PHARMA
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