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A method of high -efficiency liquid color spectrum detection method of Lidiastan

A high-performance liquid chromatography and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of small separation degree and long analysis time of rivaroxaban S isomer and R isomer, and achieve Accurate and reliable detection results, short analysis time, and easy operation

Active Publication Date: 2016-05-25
CHENGDU BAIYU PHARMA CO LTD
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AI Technical Summary

Problems solved by technology

[0006] At present, in the prior art, long and expensive chromatographic columns are used to analyze and detect the content of isomers in rivaroxaban; for example, Chinese patent CN103217492A discloses an optical isomer of rivaroxaban The separation determination method, which uses a length of 250mm IC chromatographic column separation and determination of rivaroxaban S isomer and R isomer, this method has a small separation degree of rivaroxaban S isomer and R isomer due to the large peak width of the chromatographic peak, and at the same time There is the problem that analysis time is long (analysis time reaches more than 17 minutes), if shortening retention time (that is, shortening analysis time) will cause the degree of separation of rivaroxaban S isomer and R isomer to be smaller (referring to CN103217492A attached to the manual image 3 ); Zhang Qianru (Zhang Qianru, Zhang Qi, Guo Xiaofeng, Guo Wenmin. Determination of Enantiomer Content in Rivaroxaban by HPLC. Chinese Pharmacist, 2014, Volume 17, Issue 10: 1629-1631.) and Susanne Roehrig (Susanne Roehrig, Alexander Straub, et al. Discovery of the Novel Antithrombotic Agent 5-Chloro-N-({(5S)-2-oxo-3-[4-(3-oxomorpholin-4-yl)phenyl]-1,3-oxazolidin-5-yl }methyl)thiophene-2-carboxamide (BAY59-7939): AnOral, DirectFactorXaInhibitor.J.Med.Chem., 2005, 48(19): 5900-5908.) also use a chromatographic column with a length of 250mm to measure Leval The content of saban isomers also has problems such as low resolution of rivaroxaban S isomer and R isomer, and long analysis time

Method used

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  • A method of high -efficiency liquid color spectrum detection method of Lidiastan
  • A method of high -efficiency liquid color spectrum detection method of Lidiastan
  • A method of high -efficiency liquid color spectrum detection method of Lidiastan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] High performance liquid chromatography detection method for rivaroxaban:

[0050] (1) Preparation of the test solution: Accurately weigh 10 mg of rivaroxaban, place it in a 50ml measuring bottle, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0051] Preparation of reference substance solution: take rivaroxaban R isomer 10mg, put it in a 50ml measuring bottle, add mobile phase to dissolve and dilute to the mark, shake well, and use it as a reference substance stock solution; accurately measure an appropriate amount, and quantitatively dilute it to prepare Each 1ml contains 0.2μg solution, as the reference solution;

[0052] Preparation of system suitability test solution: take rivaroxaban 10mg, put it in a 50ml measuring bottle, add mobile phase to dissolve and dilute to the mark, and shake well to obtain a rivaroxaban solution; take 0.25ml of the reference stock solution, put it in In a 25ml measuring bottle, dilute ...

Embodiment 2

[0071] Except that the mobile phase was changed to acetonitrile-water (40%:60%, volume ratio) in the detection conditions, other steps and conditions were the same as in Example 1.

[0072] According to the above detection conditions, take 20 μl of the system suitability test solution and inject it into the liquid chromatograph, record the chromatogram, see figure 2 And table 2; Get reference substance solution 20 μ l and inject liquid chromatograph, adjust detection sensitivity, make the main component chromatographic peak height be about 10% of full scale; Accurately measure each 20 μ l of need testing solution and reference substance solution, inject respectively Liquid chromatograph, record chromatogram, calculate the content of rivaroxaban R isomer in the test sample with peak area by external standard method is 0.02%.

[0073] Table 2, the separation effect of rivaroxaban enantiomers under the conditions of Example 2

[0074]

[0075] The results show that the detec...

Embodiment 3

[0077] Except that the mobile phase was changed to acetonitrile-water (60%:40%, volume ratio) in the detection conditions, other steps and conditions were the same as in Example 1.

[0078] According to the above detection conditions, take 20 μl of the system suitability test solution and inject it into the liquid chromatograph, record the chromatogram, see image 3 And table 3; Get 20 μ l of reference substance solution and inject liquid chromatograph, adjust detection sensitivity, make the main component chromatographic peak height be about 10% of full scale; Accurately measure each 20 μ l of need testing solution and reference substance solution, inject respectively Liquid chromatograph, record chromatogram, calculate the content of rivaroxaban R isomer in the test sample with peak area by external standard method is 0.02%.

[0079] Table 3, the separation effect of rivaroxaban enantiomers under the conditions of Example 3

[0080]

[0081] The results show that the dete...

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Abstract

The invention discloses a high performance liquid chromatography (HPLC) detection method of Rivaroxaban. The method comprises the following steps: a. preparing a test solution; b. preparing a reference solution; c. respectively detecting the test solution and the reference solution by adopting HPLC, wherein the detection conditions are as follow: the stationary phase of a chromatographic column is silica gel which is coated with amylose-tri ((S)-alpha-methyl phenyl carbamate) on the surface, the mobile phase of the chromatographic column is acetonitrile-water, the flow velocity is 0.5-1.5ml / min, the column temperature is 10-40 DEG C, and the detection wave length is 200nm-300nm. After the detection method is used, the degree of separation of Rivaroxaban and Rivaroxaban R isomer is more than 3.0, and more theoretical plates are available, so that the detection result accuracy is effectively prevented from being influenced by the interference of all components; furthermore, the detection method has the advantages of being accurate and reliable in detection results, short in analysis time, low in cost, simple and convenient in operation, etc.

Description

technical field [0001] The invention relates to a high performance liquid chromatography detection method for rivaroxaban. Background technique [0002] Rivaroxaban (Rivaroxaban), molecular formula: C 19 h 18 ClN 3 o 5 S, the chemical name is 5-chloro-nitrogen-({(5S)-2-oxo-3-[4-(3-oxo-4-morpholinyl)phenyl]-1,3-oxazolidine-5- Base} methyl)-2-thiophene-carboxamide, its chemical structure is as shown in formula A; Rivaroxaban is a new oral anticoagulant drug, and the rivaroxaban drug that has been approved for listing currently has Bayer Healthcare Rivaroxaban tablets (trade name: Xarelto) produced by the joint-stock company. [0003] [0004] The R isomer of rivaroxaban is the optical isomer (enantiomer) of rivaroxaban (ie, the S isomer of rivaroxaban), which will inevitably occur during the preparation of rivaroxaban. The R isomer of rivaroxaban exists at the same time; however, clinical studies have shown that the R isomer of rivaroxaban is much less effective than ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 孙毅魏农农陈明霞
Owner CHENGDU BAIYU PHARMA CO LTD
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