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Analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium

A technique for analyzing pitavastatin calcium and its analysis method, which is applied in the analytical field of quantitative detection of nitrogen and oxygen impurities in pitavastatin calcium, and can solve problems such as poor qualitative and quantitative detection and monitoring of nitrogen and oxygen impurities

Pending Publication Date: 2022-02-22
XUZHOU WANBANG JINQIAO PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of its warning structure, nitrogen and oxygen impurities need to be effectively qualitatively and quantitatively detected and monitored to ensure drug safety. However, there is currently no analytical method for qualitatively and quantitatively detecting and monitoring nitrogen and oxygen impurities.

Method used

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  • Analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium
  • Analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium
  • Analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] High performance liquid chromatography conditions:

[0051]The chromatographic column is a Welch Ultimate XB-C18 chromatographic column (250mm*4.6mm, 5μm), using dilute acetic acid buffer solution with a pH of 3.8 adjusted with sodium acetate solution and acetonitrile as mobile phase A and mobile phase B respectively, and the detection wavelength is 255nm. The flow rate is 1.0ml / min, the column temperature is 40°C, the injector temperature is 4°C, the injection volume is 10μl, and the gradient elution is performed according to the following table:

[0052] time A B 0 65 35 10 65 35 15 10 90 20 10 90 21 65 35 35 65 35

[0053] Sample preparation:

[0054] Pitavastatin calcium control solution: Weigh the reference substance, and dilute to the mark with a diluent to obtain a pitavastatin calcium control solution containing about 0.5 mg of pitavastatin calcium per 1 ml.

[0055] Pitavastatin calcium test solution: take th...

Embodiment 2

[0066] High performance liquid chromatography condition is the same as embodiment 1.

[0067] Sample preparation: use the blank mobile phase as the blank solvent for detection.

[0068] Experimental operation: Take 10 μl of blank solvent and inject, record the chromatogram.

[0069] The blank solvent selected by the inventors has been used to study the present invention. In the mobile phase chromatogram, there are no significant interference peaks near the peak positions of the main peak pitavastatin calcium and nitrogen and oxygen impurities. It is proved that the blank solvent does not interfere with the present invention.

Embodiment 3

[0071] High performance liquid chromatography condition is the same as embodiment 1.

[0072] Sample preparation:

[0073] Detection limit solution: a solution with a signal-to-noise ratio of nitrogen and oxygen impurities of about 3:1.

[0074] Limit of quantitation solution: a solution with a signal-to-noise ratio of nitrogen and oxygen impurities of about 10:1.

[0075] Test operation: Take 10 μl each of the detection limit solution and the quantification limit solution to inject samples respectively, and record the chromatogram. The inventor verified the detection limit and quantitative limit of nitrogen and oxygen impurities, and the results are shown in Table 2.

[0076] Table 2 Detection limit, limit of quantitation test result

[0077]

[0078] It can be seen from Table 2 that the finally determined detection limit and quantitative limit of nitrogen and oxygen impurities are very low, which proves that the nitrogen and oxygen impurities in pitavastatin calcium of...

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Abstract

The invention discloses an analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium. The analysis method adopts a high performance liquid chromatography, and performs qualitative and quantitative analysis on the nitrogen and oxygen impurities in the pitavastatin calcium by screening the detection wavelength, the mobile phase pH, a buffer salt type, gradient elution conditions, the sample injector temperature, the column temperature and the sample injection amount, and methodological verification is carried out. According to the method, nitrogen and oxygen impurities in the pitavastatin calcium can be effectively separated, qualitatively and quantitatively detected, and the analysis method is high in specificity and sensitivity, has a good linear curve in a low concentration range, is not influenced by personnel and instruments, has high repeatability and accuracy, and is stable and reliable.

Description

technical field [0001] The invention belongs to the field of chemical drug analysis methods, in particular to an analysis method for quantitatively detecting nitrogen and oxygen impurities in pitavastatin calcium. Background technique [0002] Pitavastatin calcium: (+)-bis{(3R,5S,6E)-7-[2-cyclopropyl-4-(4-fluorophenyl)quinolin-3-yl]-3,5- Dihydroxy-6-heptenoic acid} calcium salt (2:1), CAS: 147526-32-7, its structural formula is as follows: [0003] [0004] Pitavastatin calcium, as a hydroxymethylglutaryl coenzyme A (HMG-CoA) reductase inhibitor, is clinically used to treat hyperlipidemia. It is the third product jointly developed by Nippon Chemical Industry Co., Ltd. and Kowa Co., Ltd. Substitute statins were registered in Japan in November 1999 and approved for marketing in July 2003. It was subsequently launched in South Korea, Thailand, China and the United States. According to the results of existing clinical trials and the comparison with similar foreign products...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74G01N30/34G01N30/30G01N30/16G01N30/60G01N30/32
CPCG01N30/02G01N30/74G01N30/34G01N30/30G01N30/16G01N30/60G01N30/32G01N2030/324
Inventor 陆海波吴晓桐郭美丽胡玉敬王冉
Owner XUZHOU WANBANG JINQIAO PHARMA
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