Detection method of impurity cis-octahydroisoindole in mitiglinide calcium

A technology of mitiglinide calcium and perhydroisoindole, which is applied in the field of medicine and achieves the effects of strong specificity, good separation effect, and reliable qualitative and quantitative analysis.

Active Publication Date: 2018-12-11
SHANDONG BOYUAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, after retrieval, there is no report on the content detection method of cis-perhydroisoindole in mitiglinide calcium

Method used

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  • Detection method of impurity cis-octahydroisoindole in mitiglinide calcium
  • Detection method of impurity cis-octahydroisoindole in mitiglinide calcium
  • Detection method of impurity cis-octahydroisoindole in mitiglinide calcium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1 Instruments and materials

[0031] 1.1 Instruments: Triple Quad4500 mass spectrometer (AB, USA), LC20A high performance liquid chromatograph (Shimadzu, Japan);

[0032] 1.2 Reagents: Methanol and acetonitrile are of mass spectrometry grade, acetic acid (chromatographic grade), and water is ultrapure water.

[0033] 2 Methods and Results

[0034] 2.1 Chromatography and mass spectrometry conditions

[0035] Chromatographic column: MGⅢC 18 (2.0×100mm, 3μm, Shiseido), flow rate: 0.1ml / min, column temperature: 40°C, injection volume: 1μl, mobile phase: acetonitrile (containing 0.1% acetic acid)-water (containing 0.1% acetic acid). The gradient elution table is shown in Table 3.

[0036] Table 3 Gradient elution table

[0037]

[0038] Ion source: electrospray ionization source (ESI), positive ion mode: select multiple reaction detection scanning (MRM) mode, spray voltage (IS) 5500V; drying gas temperature 550 ° C; atomization gas (Gas1) 50psi; auxiliary gas (Gas2 ...

Embodiment 2

[0066] Embodiment 2: the detection of actual sample

[0067] 1) Get the former medicine of mitiglinide calcium, dissolve or constant volume with methanol, be mixed with the solution that contains 0.5mg mitiglinide calcium in 1ml, as need testing solution;

[0068] 2) Take the test solution prepared in step 1), adopt the same instruments and reagents as in Example 1, and carry out LC-MS / MS detection according to the chromatographic and mass spectrometry conditions shown in step 1) 2.1.

[0069] 3) According to the standard curve obtained in Example 1, find out the impurity cis-perhydroisoindole content in mitiglinide calcium.

[0070] Adopt above-mentioned method to detect three batches of samples, the result is as follows:

[0071] Table 8 Test results

[0072] Sample lot number

[0073] .

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Abstract

The invention discloses a detection method of impurity cis-octahydroisoindole in mitiglinide calcium. The detection method takes MG IIIC18 as a chromatographic column, and adopts an LC-MS / MS detectionmethod to conduct qualitative and quantitative analysis on cis-octahydroisoindole in mitiglinide calcium, and meanwhile, the methodology validation is conducted. The experiment proves that the methodhas the advantages of being high in specificity, rapid, sensitive and precise. The invention firstly builds up the quantitative and qualitative method of impurity cis-octahydroisoindole in mitiglinide calcium, the quality of mitiglinide calcium can be conveniently controlled, and accordingly the drug safety use of mitiglinide calcium is improved.

Description

technical field [0001] The invention relates to a detection method of cis-perhydroisoindole, an impurity in mitiglinide calcium, and belongs to the technical field of medicine. Background technique [0002] Miglinide Calcium (mitiglinide Calcium) is an ATP-dependent potassium ion channel blocker developed by KISSEIPHARMACEUTICAL. It was first launched in Japan in April 2004, and launched in South Korea in 2006. The original research product has been approved for marketing in China, 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. Hypoglycemia, which has obvious advantages over other traditional hypoglycemic drugs, can be used as a first-line diabetes treatment drug and has a broad market prospect. [0003] Cis-perhydroisoindole is not only the reaction material of mitigli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 王晓丹袁恺孙庆伟杨上任苏曼
Owner SHANDONG BOYUAN PHARM CO LTD
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