A kind of detection method of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride

A technology of methyl isoquinoline sulfonate and ethyl isoquinoline sulfonate, which is applied in the detection field of some impurities, can solve the problems such as difficulty in identifying the content of 5-isoquinoline sulfonic acid, and achieve the effect of good stability

Active Publication Date: 2021-06-29
SHANDONG INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
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Problems solved by technology

[0009] Aiming at the problem that the content of 5-isoquinolinesulfonic acid in fasudil hydrochloride is difficult to identify, the invention provides a kind of methyl 5-isoquinolinesulfonate and hexyl 5-isoquinolinesulfonate in fasudil hydrochloride identification method

Method used

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  • A kind of detection method of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride
  • A kind of detection method of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride
  • A kind of detection method of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 specificity experiment

[0030] (1) Blank solution: Take methanol as the blank solution;

[0031] (2) Preparation of the test solution: Accurately weigh about 12.5 mg of the sample of fasudil hydrochloride, put it in a 10 mL measuring bottle, add methanol and dilute to the mark;

[0032] (3) Preparation of the control solution: Accurately weigh about 10 mg each of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate, and quantitatively dilute with methanol to make 5-isoquinolinesulfonate containing 5-isoquinolinesulfonate per 1 mL A solution of about 5ng each of methyl ester and ethyl 5-isoquinolinesulfonate;

[0033] (4) Preparation of standard-added test solution: Accurately weigh about 12.5 mg of Fasudil hydrochloride sample, put it in a 10 mL measuring bottle, add standard solution and dilute to the mark (the content of each reference substance is about 5 ng / mL) .

[0034] (5) Precisely measure 1 µL each of the blank solvent, the test sol...

Embodiment 2

[0038] Embodiment 2 precision experiment

[0039] Preparation of the control solution: Accurately weigh about 10 mg (9.81 mg and 10.23 mg) of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate, and quantitatively dilute with methanol to make 5- A solution of about 5 ng each of methyl isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate;

[0040] Precisely measure 1 µL of the reference solution, inject it into the liquid mass spectrometer, record the chromatogram, inject 6 consecutive samples, and count the RSD values ​​of the retention time and peak area for 6 times to investigate the precision of the method. The test results are shown below surface;

[0041] Table 1 Results of the applicability test of the verification system for 5-isoquinolinesulfonate methyl ester and 5-isoquinolinesulfonate ethyl ester

[0042]

[0043] Verification requirements: RSD of retention time and peak area shall not exceed 5.0%.

[0044] Conclusion: From the above test resul...

Embodiment 3

[0045] Embodiment 3 linear relationship experiment

[0046]Preparation of linear solution: Accurately weigh 10.38 mg and 9.56 mg of methyl 5-isoquinoline sulfonate and ethyl 5-isoquinoline sulfonate in the same volumetric flask, and quantitatively dilute with methanol so that each 1 mL contains about 200 ng, A series of solutions of 100ng, 50ng, 20ng, 10ng, 5ng, and 2ng were used as linear solutions of 4000%, 2000%, 1000%, 400%, 200%, 100%, and 40% concentration of the control solution.

[0047] Precisely measure 1 µL of each linear solution, inject it into the liquid mass spectrometer respectively, record the chromatogram, and take the concentration as the abscissa ( X ), the peak area is the ordinate ( Y ) for linear regression. The test results are shown in the table below.

[0048] Table 2 5-isoquinolinesulfonate methyl ester, 5-isoquinolinesulfonate ethyl ester inspection method validation linear relationship test results

[0049]

[0050] Verification requirements...

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Abstract

The invention belongs to the field of medicinal chemistry, and in particular relates to a LC-MSMS method for determining the content of methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride. HPLC solves the problem that methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate cannot be simultaneously determined under single liquid phase conditions, and the mobile phase has great damage to the chromatographic column, and the chromatographic column is not durable, resulting in poor method reproducibility . LC‑MS has high detection sensitivity and can detect two components at the same time. The method has good durability, high accuracy, shortens analysis time and improves detection efficiency.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to the detection of some impurities in fasudil hydrochloride. Background technique [0002] Fasudil hydrochloride, the published assay method is the HPLC method (see Chinese Pharmacopoeia 2015 edition two), specifically as follows: the relevant substances are taken from this product, dissolved in mobile phase and diluted to make a solution containing about 0.3mg per 1ml , as need testing solution; Precision measures 1ml, puts in 100ml measuring bottle, is diluted to scale with mobile phase, shakes up, as contrast solution. Precisely measure 5ml of the control solution, put it in a 100ml measuring bottle, dilute to the mark with mobile phase, shake well, and use it as a sensitivity solution. Octadecylsilane bonded silica gel is used as filler, and 1.0% (v / v) triethylamine aqueous solution (adjusting the pH value to 7.0 with phosphoric acid)-methanol (50:50) (v / v) is used as mobile phase...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/047
Inventor 巩丽萍郭常川邢晟杭宝建张迅杰赵艳霞
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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