Method for detecting related substances in aprepitant by high performance liquid chromatography

A technology of high performance liquid chromatography and related substances, which is applied in the field of high performance liquid chromatography to detect related substances in aprepitant, which can solve the problems of high detection cost, sensitive pH value, shortened service life of chromatographic columns, etc., and achieve accurate detection results , High resolution, small value effect

Active Publication Date: 2015-08-26
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] At present, when detecting related substances in aprepitant, in order to achieve good resolution and detection effect, it is often necessary to add trifluoroacetic acid, sodium lauryl sulfate and other ion pairs that are very harmful to the chromatographic column in the mobile phase. Reagents (Yu Li, Gu Hui, Chao Ruobing. Research on related substances in aprepitant. Journal of Pharmaceutical Analysis. 2013, 33 (8) and Chinese patent CN 103760257 A.), trifluoroacetic acid, sodium lauryl sulfate, etc. The reagent will cause irreversible damage to the chromatographic column, and this type of ion pair reagent is difficult to wash off from the chromatographic column, which will greatly shorten the service life of the chromatographic column, and the detection cost is high. At the same time, this type of ion pair reagent is sensitive to pH , high precision is required when preparing the mobile phase, otherwise it will directly affect the repeatability and reproducibility of the experiment, and the practical application value of this detection method is also very small

Method used

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  • Method for detecting related substances in aprepitant by high performance liquid chromatography
  • Method for detecting related substances in aprepitant by high performance liquid chromatography
  • Method for detecting related substances in aprepitant by high performance liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0073] The method for the detection of related substances in aprepitant by high performance liquid chromatography of the present invention:

[0074] Chromatographic column: Waters Symmetry C18, 4.6mm×250mm, 5μm;

[0075] Diluent: acetonitrile-water (1:1);

[0076] Mobile phase A: acetonitrile-buffer (20:80), mobile phase B: acetonitrile-buffer (80:20);

[0077] Buffer: 1.96g phosphoric acid, 0.34g tetrabutylammonium hydrogensulfate, 1.0g potassium dihydrogenphosphate, dissolved in 1000ml water;

[0078] Elution was carried out according to the following gradient elution procedure, see Table 1:

[0079] Table 1, gradient elution program of the present invention

[0080] time (minutes)

[0081] Detection wavelength: 215nm;

[0082] Column temperature: 35°C; flow rate: 1.0ml / min;

[0083] System suitability test:

[0084] Take 5mg each of the relevant substances A-F, B, C, and D, add diluent to dissolve and set the volume to 100ml, shake well, and use it as a mixe...

Embodiment 2

[0102]In addition to changing the mobile phase to "mobile phase A: acetonitrile-buffer (10:90), mobile phase B: acetonitrile-buffer (90:10); buffer: 1.96g phosphoric acid, 0.34g tetrabutylammonium bisulfate, 1.0g potassium dihydrogen phosphate, be dissolved in 1000ml water ", other steps, condition, gradient elution procedure etc. are all identical with embodiment 1.

Embodiment 3

[0104] Except changing the column temperature and flow rate to "column temperature 30°C; flow rate 0.8ml / min", other steps, conditions, gradient elution procedures, etc. are the same as in Example 1.

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Abstract

The invention discloses a method for detecting related substances in aprepitant by high performance liquid chromatography. The method comprises the following steps: a. preparing a test solution; b. preparing a reference substance solution; c. respectively detecting the test solution and the reference substance solution by high performance liquid chromatography; and d. calculating the content of the related substances in a test article by peak area by virtue of an external standard method. By adopting a specific flowing phase and a gradient elution program, the related substances in aprepitant can be detected, the degree of separation of the main peak is high, the numerical value of a tailing factor of the main peak is small, and the degree of separation of impurity compounds is high. The related substances in aprepitant are relatively comprehensively detected and controlled, and the test result is relatively accurate and reliable. Furthermore, as no ion-pairing agent which poses great harm to the chromatographic column such as trifluoroacetic acid, lauryl sodium sulfate and the like is added, and according to the detection method disclosed by the invention, harm to the chromatographic column is slight.

Description

technical field [0001] The invention relates to a method for detecting related substances in aprepitant by high performance liquid chromatography. Background technique [0002] The chemical name of aprepitant is: 5-[[(2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3- (4-fluorophenyl)-4-morpholine]methyl]-1,2-dihydro-3H-1,2,4-triazol-3-one, molecular formula: C 23 h 21 f 7 N 4 o 3 , molecular weight: 534.43, and the structural formula is as follows; the aprepitant products that are now on the market include aprepitant capsules (aprepitant capsules are recorded in the "Registration Standards for Imported Drugs" of the State Food and Drug Administration, standard number: JX20050253). [0003] [0004] In aprepitant products, there are often many different related substances: impurity compounds A-1, A-F, B, B', C, C', D, D', etc.; the existence of these impurity compounds will seriously It affects the quality control and drug safety of aprepitant products, so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 孙毅宋务雄
Owner CHENGDU BAIYU PHARMA CO LTD
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