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High-performance liquid chromatography method for clopidol related substances

A technology of high performance liquid chromatography and chlorpyridine, applied in the field of drug analysis, can solve problems such as unfavorable process research, inability to quantify impurities, poor sensitivity, etc., and achieve the effects of high economic benefit, good specificity and fast analysis speed

Active Publication Date: 2018-04-13
JIANGSU TIANHE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the existing thin-layer chromatography technology has significant deficiencies in process research and quality control. The existing thin-layer chromatography technology has poor specificity, and impurities are generally shown as spots, which is not conducive to the development of process research. The sensitivity is poor and impurities cannot be quantified. The limit of 1.0% confirmed the extensiveness and limitations of thin-layer chromatography in the control of related substances
[0006] In summary, there are significant deficiencies in the prior art in the detection of related substances of chlorhydrin

Method used

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  • High-performance liquid chromatography method for clopidol related substances
  • High-performance liquid chromatography method for clopidol related substances
  • High-performance liquid chromatography method for clopidol related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: to the detection of known impurity

[0039] Test equipment and chromatographic conditions:

[0040] Agilent 1260 HPLC

[0041] Chromatographic column: Dr. Maisch C18 column (250mm×4.6mm, 5μm)

[0042] Mobile phase: pH7.0 phosphate buffer-methanol mixture, the volume ratio of the two is 80:20

[0043] The flow rate was set at 1.0 mL / min, the column temperature was set at 30° C., and the detection wavelength was 254 nm.

[0044] Experimental steps:

[0045] (1) Sample preparation:

[0046] Impurity A solution: Take about 10 mg of impurity A, dissolve it with mobile phase, and dilute it to a solution containing about 4 μg / mL of impurity A.

[0047] Pyridine solution: take 10 mg of cloxyridine, put it in a 10 mL measuring bottle, add 100 mL of methanol and 100 μL of 1 mol / L sodium hydroxide solution, dissolve it by ultrasonic, and make up to volume with methanol.

[0048] The mixing of cloxyridine and known impurity: get impurity A solution 1mL and cloxy...

Embodiment 2

[0051] Embodiment 2: to the detection of unknown impurity

[0052] Test equipment and chromatographic conditions:

[0053] Agilent1260 High Performance Liquid Chromatograph

[0054]Chromatographic column: Dr.MaischC18 column (250mm×4.6mm, 5μm)

[0055] Mobile phase: pH7.0 phosphate buffer-methanol mixture, the volume ratio of the two is 80:20

[0056] The flow rate was set at 1.0 mL / min, the column temperature was set at 30° C., and the detection wavelength was 254 nm.

[0057] Experimental steps:

[0058] (1) Sample preparation:

[0059] Sample preparation: Take 10 mg of crude pyridinium and put it in a 10 mL measuring bottle, add 100 mL of methanol and 100 μL of 1mol / L sodium hydroxide solution, ultrasonically dissolve, set methanol to volume, accurately measure 2 mL of the solution, put it in a 10 mL measuring bottle, and set the mobile phase capacity, as the test solution.

[0060] (2) Detection: Take the above-mentioned test solution, inject 20 μL, and record the ch...

Embodiment 3

[0062] Embodiment 3: to the purity detection of sample

[0063] Test equipment and chromatographic conditions:

[0064] Agilent1260 High Performance Liquid Chromatograph

[0065] Chromatographic column: Dr.MaischC18 column (250mm×4.6mm, 5μm)

[0066] Mobile phase: pH7.0 phosphate buffer-methanol mixture, the volume ratio of the two is 80:20

[0067] The flow rate was set at 1.0mL / min, the column temperature was set at 30°C, and the detection wavelength DAD was scanned at full wavelength.

[0068] (1) Sample preparation:

[0069] Undamaged: Take 10 mg of chlorhydrin sample and put it in a 10 mL measuring bottle, add a small amount of methanol and 100 μL of 1 mol / L sodium hydroxide solution, ultrasonically dissolve, set methanol to volume, accurately measure 2 mL of the solution, put it in a 10 mL measuring bottle, and set the mobile phase container, as an undisturbed solution.

[0070] Acid destruction: Take 100mg of chlorhydrin sample, accurately weigh it, put it in a 10m...

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Abstract

The invention belongs to the technical field of medicine analysis and particularly relates to a high-performance liquid chromatography method for clopidol related substances. The method includes: taking octadecyl silane serves as a stationary phase, taking mixed liquid of phosphate buffer (or acetate or borate) with pH of 3.0-8.0 and methyl alcohol (or acetonitrile or tetrahydrofuran) as a mobilephase, injecting into a high-performance liquid chromatograph under conditions that column temperature is 20-60 DEG C, sample injection quantity is 5-50microlitre and flow velocity is 0.5-2mL / min, andperforming sample analysis in a wavelength range of 200-380nm. The high-performance liquid chromatography method is high in separation efficiency, quick in analysis and high in detection sensitivity,clopidol quality is controlled by detection of the content of impurities in clopidol, and accordingly product stability and quality can be better controlled.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high-performance liquid chromatography detection method for clonazine-related substances. Background technique [0002] Clohydroxypyridine is a hydroxypyridine anticoccidial drug, which is one of the most widely used anticoccidiostats in China. It is effective against various chicken coccidia and is usually mixed in animal feed for continuous use. Pyridine premix. [0003] The existing technology for the determination of related substances of cloxyridine bulk drug only has the standards of the Chinese Veterinary Pharmacopoeia, as follows: [0004] Take 0.10g of this product, put it in a 10mL measuring bottle, add about 5mL of methanol, mix well, add 2mL of sodium hydroxide solution (1→50), ultrasonically dissolve it completely, dilute to the mark with methanol, shake well, and use it as the test sample Solution; accurately measure an appropriate amount, quan...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈龙赵云德刘磊黄正帅孙浩
Owner JIANGSU TIANHE PHARMA CO LTD
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