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Derivatized HPLC-UV method for the determination of mesylate in methanesulfonic acid

A technology of mesylate and methanesulfonic acid is applied in the field of derivatization HPLC-UV method for the determination of mesylate in methanesulfonic acid, and the derivatization HPLC-UV method for the determination of mesylate, which can solve problems such as low sensitivity and the like , to achieve the effect of good stability, good linear relationship and good specificity

Active Publication Date: 2020-04-07
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, pentafluorothiophenol is easily oxidized and will interfere with HPLC detection
While thiocyanate derivatization produces multiple derivatized products, resulting in low sensitivity

Method used

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  • Derivatized HPLC-UV method for the determination of mesylate in methanesulfonic acid
  • Derivatized HPLC-UV method for the determination of mesylate in methanesulfonic acid
  • Derivatized HPLC-UV method for the determination of mesylate in methanesulfonic acid

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Experimental program
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Effect test

preparation example Construction

[0039] 1.3. Solution preparation

[0040] Preparation of mesylate stock solution and series of mixed stock solutions:

[0041] Methyl methanesulfonate stock solution: Take about 25mg of methyl methanesulfonate, weigh it accurately, place it in a 25mL measuring bottle, dilute to the mark with N,N-dimethylacetamide, and shake well.

[0042] Ethyl methanesulfonate stock solution: take about 25mg of ethyl methanesulfonate, weigh it accurately, put it in a 25mL measuring bottle, dilute to the mark with N,N-dimethylacetamide, and shake well.

[0043] Series of mesylate mixed stock solutions: Precisely pipette equal amounts of methyl methanesulfonate stock solution and ethyl methanesulfonate stock solution, put them in a 10mL measuring bottle, add N,N-dimethylacetamide to scale, diluted into a series of mixed stock solutions containing the same concentration of methyl methanesulfonate and ethyl methanesulfonate (1.5, 2.5, 5, 10, 25, 100, 250 μg / mL).

[0044] Preparation of derivati...

Embodiment 1

[0049] The comparison of embodiment 1 derivatization reagent

[0050] Precisely pipette three times, each time 100 μL of mesylate mixed stock solution with a concentration of 250 μg / mL, place them in three 5 mL volumetric flasks, add 200 μL of water and 500 μL of dithiocarbamate derivatization test in sequence solution, add N,N-dimethylacetamide to dilute to the mark, vortex for 10s, and shake well. Heated in a water bath at 80°C for 1 hour, took it out and allowed it to cool to room temperature, filtered, and injected 20 μL into HPLC-DAD for sample analysis.

[0051] HPLC-DAD conditions: Shimadzu LC 20AT liquid chromatograph (including online vacuum degasser, binary gradient pump, autosampler, column oven, DAD detector and LC-solution chromatographic workstation); chromatographic conditions are the same as those in 1.4 Description; DAD scanning wavelength: 200-400nm.

[0052] The ultraviolet maximum absorption wavelengths of the derivatization products generated by the thre...

Embodiment 2

[0053] Identification of Example 2 Derivatization Products

[0054] Precisely pipette 100 μL of mesylate mixed stock solution with a concentration of 250 μg / mL, place it in a 5 mL volumetric flask, add 200 μL of water and 500 μL of DDTC derivatization test solution in turn, add N,N-dimethylacetamide to dilute to Scale, vortex for 10 s, and shake well. Heated in a water bath at 80°C for 1 hour, took it out and allowed it to cool to room temperature, filtered, and injected 20 μL into HPLC-MS for sample analysis.

[0055] HPLC-MS conditions: Agilent 6224-TOF high performance liquid chromatography-precision mass spectrometry; Chromatographic conditions are the same as described in 1.4; Mass spectrometry ion source: ESI (+); Scanning range: m / z 90-230; Dry gas (N 2 ) flow rate: 8.0L / min; drying gas temperature: 325°C; capillary voltage: 3.5kV; resolution: 200,000.

[0056] High-performance liquid chromatography precision mass spectrometry results are: the measured molecular weigh...

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Abstract

The invention discloses a method for measuring methanesulfonate in methanesulfonic acid by a derivatization HPLC-UV method. The method uses a dithiocarbamates derivatization reagent for derivatization of methanesulfonate to generate product having strong absorption capacity in an ultraviolet light zone; a derivative reaction liquid is taken as a sample introduction sample, based on an anti-phase high-performance liquid chromatography principle, the derivatization products of the methanesulfonate are separated and determined, so that qualitative or quantitative determination can be carried out on the methanesulfonate. According to the invention, the methanesulfonate and the dithiocarbamates derivatization reagent are subjected to a reaction, the generate product has UV absorption characteristic, and the invention establishes the simple and general method for measuring methanesulfonate in methanesulfonic acid by the derivatization HPLC-UV method. The method has good specificity and good sensitivity through results by methodology validation.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to a method for determining mesylate by a derivatization HPLC-UV method, in particular to a method for determining mesylate in methanesulfonic acid by a derivation 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 [1,2] . In recent years, with the gradual improvement of genotoxic impurity regulations, the United States Food and Drug Administration (FDA) and the European Medicines Agency (EMEA) have increasingly strict regulatory requirements for genotoxic impurities [3,4] . If the genotoxic impurities in the drug are not properly controlled, it may lead to clinical hidden dangers, and it will also affect the time to market new drugs. Therefore, in the drug production process, the control ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 郑枫柳文媛周洁冯锋
Owner CHINA PHARM UNIV
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