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Method for measuring crystal form proportion in compound in quantitative mode

A technique for quantitative determination of compounds, applied in the field of quantitative determination of crystal form ratios in compounds, can solve problems such as methods for determining the proportion of different crystal forms of compounds that have not yet been seen, and achieve the effects of easy promotion, simple operation, and low cost

Active Publication Date: 2013-01-09
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] There is no method for quantitatively determining the proportion of different crystal forms in a compound by using infrared absorption spectroscopy

Method used

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  • Method for measuring crystal form proportion in compound in quantitative mode
  • Method for measuring crystal form proportion in compound in quantitative mode
  • Method for measuring crystal form proportion in compound in quantitative mode

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0070] c. The closer the correlation coefficient R of the relationship curve is to 1, the better the linearity of the relationship curve and the higher the accuracy of the method. Example 1 Determination of the ratio of linezolid crystalline form II to crystalline form IV (quantitative wavenumbers are 852 ± 2cm -1 With 825±2cm -1 )11 respectively select the quantitative wavenumbers of linezolid crystal form II and linezolid crystal form IV

[0071] 1.1.1 Weigh an appropriate amount of pure linezolid crystal form II, grind to form particles smaller than 1 micron, and then mix these particles with potassium bromide powder at a ratio of 1:200 (mass ratio), and mix the mixed The powder was pressed into a tablet to form a thin sheet sample with a thickness of about 0.5-1 mm. The blank potassium bromide tablet was used as a background for reference, and infrared scanning was carried out 15 times to obtain the crystal form II of linezolid at 4000-400 cm. -1 For infrared absorption ...

Embodiment 2

[0081] Example 2 Determination of the ratio of linezolid crystal form II to crystal form IV (quantitative wavenumbers are 1445 ± 2 cm -1 With 1425±2cm -1 )

[0082] 2.1 Select the quantitative wavenumbers of Linezolid Form II and Linezolid Form IV respectively

[0083] According to the method in 1.1.1, the crystal form IV of linezolid was obtained at 4000-400cm -1 Infrared absorption band within the range; according to the method in 1.1.2, the crystal form IV of linezolid was obtained at 4000~400cm -1 range of infrared absorption bands.

[0084] Comparing the infrared absorption band of the crystal form II with the infrared absorption band of the crystal form IV, it is found that the crystal form II is at 1445±2cm -1 There is a sharp absorption peak at , while the crystal form IV has no absorption peak at this place; the crystal form IV is at 1425±2cm -1 There is a sharp absorption peak at , while the crystal form II has no absorption peak at this position. Therefore, ch...

Embodiment 3

[0092] Example 3 Determination of the ratio of linezolid crystalline form II to crystalline form IV (quantitative wavenumbers are 679±2cm -1 With 661±2cm -1 )

[0093] 3.1 Select the quantitative wavenumbers of Linezolid Form II and Linezolid Form IV respectively

[0094] According to the method in 1.1.1, the crystal form IV of linezolid was obtained at 4000-400cm -1Infrared absorption band within the range; according to the method in 1.1.2, the crystal form IV of linezolid was obtained at 4000~400cm -1 range of infrared absorption bands.

[0095] Comparing the infrared absorption band of the crystal form II with the infrared absorption band of the crystal form IV, it is found that the crystal form II is at 679±2cm -1 There is a sharp absorption peak at , while the crystal form IV has no absorption peak at this place; the crystal form IV is at 661±2cm -1 There is a sharp absorption peak at , while the crystal form II has no absorption peak at this position. Therefore, ch...

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Abstract

The invention relates to a method for measuring crystal form proportion in a compound in a quantitative mod by using infrared spectroscopy, which comprises the following steps: respectively selecting two crystal forms at 'quantitative wave number pairs' of certain characteristic absorption peak in the compound to be measured, respectively determining the absorbance of the object to be measured with known crystal form proportion at the position of 'quantitative wave number pairs', and establishing a 'crystal form ratio-absorbance ratio' relation curve, thereby the proportion of crystal form to be measured can be conveniently measured in the quantitative mode. According to the invention, the proportion of a crystal form II and a crystal form IV in linezolid can be measured, the relative error between the measured value and practical value is small. The quantitative measurement on the crystal form proportion has high specialization and accuracy, the cost is low and the operation is simple.

Description

technical field [0001] The invention relates to a method for quantitatively determining the ratio of different crystal forms in a compound by infrared spectroscopy, in particular to a method for determining the ratio of crystal form II and crystal form IV in linezolid. Background technique [0002] More than one crystal form often exists for the same compound. The physical properties, biological activities and applications of different crystal forms may be different. For example, the polymorphic form of a drug may affect the quality, safety and stability of the drug, the type of crystal form and the ratio between different crystal forms, and may also affect the bioavailability of the drug. Therefore, it is necessary to determine the proportion of different crystal forms in the compound. [0003] However, it is difficult to quantitatively determine the proportion of crystal forms. Because the chemical properties of different crystal forms in the same compound are basically...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N21/3563
Inventor 雷海燕
Owner CHONGQING HUAPONT PHARMA