Detecting method of impurity succinic acid in S-benzylsuccinic acid

A benzyl succinic acid and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve strong specificity, good separation effect, and improve the effect of drug safety

Active Publication Date: 2019-04-05
SHANDONG BOYUAN PHARM CO LTD
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  • Description
  • Claims
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  • Detecting method of impurity succinic acid in S-benzylsuccinic acid
  • Detecting method of impurity succinic acid in S-benzylsuccinic acid
  • Detecting method of impurity succinic acid in S-benzylsuccinic acid

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[0031] Example 1

[0032] 1 Instruments and materials

[0033] 1.1 Instrument: Waters Arc 2489 high performance liquid chromatograph (Waters, USA);

[0034] 1.2 Reagents: methanol (chromatographic grade), phosphoric acid (chromatographic grade), water is ultrapure water.

[0035] 2 methods and results

[0036] 2.1 Chromatographic conditions

[0037] Chromatographic column: Agilent ZORBAX SB-CN chromatographic column (4.6×250mm, 5μm), column temperature: 35°C, injection volume: 40μl;

[0038] Mobile phase A: methanol-water (containing 0.1% phosphoric acid)=5:95, mobile phase B: methanol-water (containing 0.1% phosphoric acid)=45:55, solvent: methanol-water=5:95; flow rate: 1.0ml / min, the gradient elution conditions are shown in Table 1.

[0039] Detector: Waters 2489 ultraviolet detector, detection wavelength: 212nm.

[0040] 2.2 Preparation of the solution

[0041] 2.21 Preparation of specific solution

[0042] Accurately weigh 31.15mg of the reference substance of succinic acid, put it in ...

Example Embodiment

[0082] Example 2: Detection of actual samples

[0083] 1) Take S-benzyl succinic acid, dissolve it in a solvent and make the volume constant, and prepare a solution containing 3 mg of S-benzyl succinic acid in 1 ml as the test solution;

[0084] 2) Take succinic acid, dissolve it with a solvent and make a constant volume, and prepare 1ml solution containing 0.003mg of succinic acid as the reference solution;

[0085] 3) Take 40μl of the test solution prepared in step 1) and the reference solution prepared in step 2) directly (separately) into the sample, using the same instruments and reagents as in Example 1, and proceed according to the chromatographic conditions shown in 2.1 HPLC detection, record the chromatogram;

[0086] 3) According to the external standard method, the content of impurity succinic acid in S-benzyl succinic acid was calculated by the peak area.

[0087] Three batches of samples were tested using the above method, and the results are shown in Table 5:

[0088] Tabl...

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Abstract

The invention discloses a detecting method of impurity succinic acid in S-benzylsuccinic acid. Agilent SB-CN is adopted as a chromatographic column, the HPLC detecting method is adopted to qualitatively and quantitatively detect the succinic acid in the S-benzylsuccinic acid, and methodology validation is conducted. The experimental results show that the method has the advantages of being high inspecificity, fast, sensitive and accurate. The qualitative and quantitative method of the impurity succinic acid in the S-benzylsuccinic acid is established for the first time, the mass of the S-benzylsuccinic acid can be conveniently controlled, and therefore drug safety of using the S-benzylsuccinic acid as an intermediate active component is improved.

Description

technical field [0001] The invention relates to a detection method of succinic acid, an impurity in S-benzylsuccinic acid, and belongs to the technical field of medicine. Background technique [0002] S-benzylsuccinic acid ((S)-2-Benzylsuccinic acid) is an important pharmaceutical intermediate, mainly used in the production of mitiglinide calcium. Miglinide Calcium is an ATP-dependent potassium ion channel blocker developed by KISSEIPHARMACEUTICAL. It was first launched in Japan in April 2004. It was launched in South Korea in 2006. In 2010, the original product was launched in China. It has been approved for marketing, and many pharmaceutical manufacturers in China have been approved for production. Miglinide calcium is clinically used to treat type 2 diabetes. Its mechanism of action is similar to that of sulfonylurea, but it works faster and has a shorter half-life. The hypoglycemia of hypoglycemia has obvious advantages over other traditional hypoglycemic drugs, and ca...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 钱振英孙庆伟闫玲玲张秀云王娜
Owner SHANDONG BOYUAN PHARM CO LTD
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