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Determination of mesylate by derivatized hplc-uv method

A mesylate and derivatization technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of lower detection sensitivity, tailing, low sensitivity, etc., and achieve good linear relationship, good specificity, and good stability Effect

Active Publication Date: 2021-06-15
ZIBO VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the products of these derivatization reagents (quaternary ammonium salts) will cause tailing due to the interaction of silanols, reducing detection sensitivity
Pentafluorothiophenol and thiocyanate are strong nucleophiles, which are used as derivatization reagents for gas chromatography-mass spectrometry (GC-MS) to determine the content of mesylate; but pentafluorothiophenol is easily oxidized, and In HPLC detection, there will be interference; and thiocyanate derivatization will produce a variety of derivatized products, resulting in low sensitivity
However, the thioamide / thioalkyl ester groups in these reagents are easily hydrolyzed with acid or base, resulting in a greatly reduced derivatization efficiency

Method used

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  • Determination of mesylate by derivatized hplc-uv method
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  • Determination of mesylate by derivatized hplc-uv method

Examples

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preparation example Construction

[0044] 3. Solution Preparation

[0045] Methyl methanesulfonate stock solution: Take about 10 mg of methyl methanesulfonate, weigh it accurately, put it in a 10ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well to get 1mg / ml.

[0046] Ethyl methanesulfonate stock solution: Take about 10 mg of ethyl methanesulfonate, weigh it accurately, put it in a 10ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well to get 1mg / ml.

[0047] Series mesylate mixed stock solution: Precisely measure the same amount of methyl mesylate stock solution and ethyl mesylate stock solution, put them in a 10ml measuring bottle, add acetonitrile to dilute to the mark, and dilute to contain the same concentration of formazan A series of mixed stock solutions of methyl sulfonate and ethyl methane sulfonate (concentrations 5, 10, 20, 30, 40, 50 μg / ml).

[0048] 2-Naphthylthiol Derivatization Solution: Take about 125mg of 2-Naphthylthiol, we...

Embodiment 1

[0053] Precisely measure 0.1ml of 50μg / ml mesylate mixed stock solution, place it in a 5ml measuring bottle, add 1.0ml of 1.0mg / ml 2-naphthylthiophenol derivatization solution and 0.10mol / L NaOH solution in sequence 0.5ml, dilute to the mark with acetonitrile, shake well, react at 80°C for 2h, let cool to room temperature, centrifuge at 10000rpm for 5min, take 20μl of the supernatant and inject it into HPLC-DAD for analysis.

[0054] HPLC-DAD conditions: instrument conditions are the same as those described in 1; chromatographic conditions are the same as those described in 4; DAD scans at 200-400nm.

[0055] The maximum absorption wavelength of the methyl methanesulfonate product is 252nm, the maximum absorption wavelength of the ethyl methanesulfonate product is 253nm, and the maximum absorption wavelength of the ethyl methanesulfonate product is selected as the detection wavelength.

Embodiment 2

[0057] Precisely measure 6 parts, each part of 0.10ml of a series of mesylate mixed stock solutions, place them in six 5ml measuring bottles, add 5.0mg / ml of 2-naphthylthiol derivatization solution 1.0ml and 0.50mol / 0.5ml of NaOH solution in L, dilute to the mark with acetonitrile, shake well, and make solutions with mesylate of 0.1, 0.2, 0.4, 0.6, 0.8, 1.0μg / ml, react at 80°C for 2h, let cool to Centrifuge at 10,000 rpm for 5 minutes at room temperature, and take 20 μl of the supernatant and inject it into HPLC-UV analysis.

[0058] Take about 100mg of imatinib mesylate, accurately weigh it, place it in a 10ml measuring bottle, dissolve it with water-acetonitrile solution (10:90, v / v) and dilute to the mark to obtain the product. Precisely measure 0.5ml, put it in a 5ml measuring bottle, add 1.0ml of 5.0mg / ml 2-naphthylthiol derivatization solution and 0.5ml of 0.50mol / L NaOH solution, dilute to the mark with acetonitrile, shake well, and React at 80°C for 2 hours, let cool...

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Abstract

The invention belongs to the technical field of drug analysis and detection, and in particular relates to a method for measuring mesylate by a derivatization HPLC-UV method. Use 2-naphthylthiol derivatization reagent to derivatize mesylate to generate a derivatized product that absorbs at 252-253nm in the ultraviolet region, and use HPLC reverse-phase partition chromatography to measure methanesulfonic acid at 252-253nm in the ultraviolet region Derivatized products of esters, so as to realize the qualitative and quantitative detection of mesylate in raw materials containing methanesulfonic acid. When adopting the assay method of the present invention to measure, imatinib mesylate and other impurities in imatinib mesylate will not interfere with the analysis, and the specificity of the method is good; the detection limit of the method is 0.03 μg / ml, the limit of quantification is 0.10 μg / ml, and the linear relationship is good; the average recovery rate is between 87.5‑102.1%, without obvious matrix interference; and the derivatized product has good stability within 6 hours.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and detection, and in particular relates to a method for measuring mesylate by a derivatization HPLC-UV method. Background technique [0002] Potential genotoxic impurities are strong mutagens and carcinogens, which can cause DNA mutation, chromosome breakage or DNA recombination, and may also lead to the occurrence of human tumors. In recent years, with the gradual improvement of genotoxic impurity regulations, the US Food and Drug Administration (FDA) and the European Medicines Agency (EMEA) have increasingly strict regulatory requirements for genotoxic impurities. If the genotoxic impurities in the drug are not properly controlled, it may lead to clinical hidden dangers and also affect the time to market of new drugs. Therefore, in the drug production process, the control of potential genotoxic impurities is very important. [0003] Mesylate is a common class of potential genotoxic impur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 徐洁
Owner ZIBO VOCATIONAL INST
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