High performance liquid chromatography detection method of Cangrelor intermediate adenosine-2-thione

A high-performance liquid chromatography and detection method technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unseen compound detection methods and other reports, and achieve accurate and reliable detection results, easy operation, and high plate number Effect

Active Publication Date: 2017-12-12
盐城锦明药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] At present, there is no relevant report on the detection method of the compound represented by formula B

Method used

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  • High performance liquid chromatography detection method of Cangrelor intermediate adenosine-2-thione
  • High performance liquid chromatography detection method of Cangrelor intermediate adenosine-2-thione
  • High performance liquid chromatography detection method of Cangrelor intermediate adenosine-2-thione

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Embodiment 1

[0041] This embodiment provides a high-performance liquid chromatography detection method for Cangrelor intermediate adenosine-2-thione, comprising the following steps:

[0042] Preparation of standard solution: Accurately weigh 0.100 g of the product adenosine-2-thione, dissolve it in 0.1 mol / L NaOH solution, and set the volume to 100 mL. Filter with a 0.45 μm microporous membrane to obtain a standard solution, and take 5 μl for injection;

[0043] The standard solution is detected by reversed-phase high-performance liquid chromatography, and the detection conditions are:

[0044] The stationary phase of the chromatographic column: silica gel with a non-polar octadecyl functional group (ODS) bonded to the surface as a filler;

[0045] Mobile phase: acetonitrile and 0.3% acetic acid aqueous solution (adjust the pH to 5.8 with triethylamine) (5.5:94.5(V:V));

[0046] Flow rate: 0.5ml / min;

[0047] Column temperature: 25°C;

[0048] Detection wavelength: 254nm;

[0049] Acc...

Embodiment 2

[0056] This embodiment provides the existing high performance liquid chromatography detection method of Cangrelor intermediate adenosine-2-thione, comprising the following steps:

[0057] Preparation of standard solution: Accurately weigh 0.010 g of the product adenosine-2-thione, dissolve it in pure water, and set the volume to 100 mL. Filter with a 0.45 μm microporous membrane to obtain a standard solution, and take 5 μl for injection;

[0058] The standard solution is detected by reversed-phase high-performance liquid chromatography, and the detection conditions are:

[0059]The stationary phase of the chromatographic column: silica gel with a non-polar octadecyl functional group (ODS) bonded to the surface as a filler;

[0060] Mobile phase: acetonitrile and phosphoric acid aqueous solution (pH=3) (5:95-30:70 (V:V) gradient elution);

[0061] Flow rate: 1ml / min;

[0062] Column temperature: 25°C;

[0063] Detection wavelength: 260nm;

[0064] According to the above de...

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Abstract

The invention discloses a high performance liquid chromatography detection method of a Cangrelor intermediate adenosine-2-thione. The high performance liquid chromatography detection method comprises the following steps: a, preparing a standard solution; b, detecting the standard solution by adopting reversed-phase high performance liquid chromatography; c, calculating the content of the adenosine-2-thione in a sample by peak area according to an external standard method. According to the detection method disclosed by the invention, the adenosine-2-thione, raw materials and other impurities can be separated well on a high performance liquid chromatograph; a linear relation is good within a range of 0.5mg / ml to 6.0mg / ml, R2 is equal to 0.9999, the average recovery rate is 102.11 percent and the RSD (Relative Standard Deviation) is 2.70 percent.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a high performance liquid chromatography detection method for Cangrelor intermediate adenosine-2-thione. Background technique [0002] Cangrelor, molecular formula: C 17 h 25 Cl 2 f 3 N 5 o 12 P 3 S 2 , CAS registration number: 163706-06-7, its chemical structure is shown in formula A; Cangrelor is a short-acting reversible inhibitor of platelet P2Y12, this drug is mainly for the prevention of adult patients in percutaneous coronary intervention (PCI) Coronary artery ramification caused by blood clotting during the procedure. As early as March 2015, the European Medicines Agency (EMA) had approved the marketing of its product name Kengrexal. On June 22, 2016, the US FDA approved the listing of Cangrelor, an antiplatelet drug injection from Medicine. [0003] [0004] Adenosine-2-thione is an important intermediate in the synthesis of Cangrelor, also known...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨子健房月邱悦王鹏吴振杨锦明
Owner 盐城锦明药业有限公司
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