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Method for measuring methanesulfonate by virtue of derivatization 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: 2018-09-21
ZIBO VOCATIONAL INST
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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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preparation example Construction

[0044] 3. Preparation of Solutions

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

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

[0047] Serial mesylate mixed stock solution: Precisely measure equal amounts of methyl methanesulfonate stock solution and ethyl methanesulfonate stock solution, place them in a 10ml volumetric flask, add acetonitrile to dilute to the mark, and dilute to contain the same concentration of methyl methanesulfonate. A series of mixed stock solutions of methyl sulfonate and ethyl methanesulfonate (concentrations 5, 10, 20, 30, 40, 50 μg / ml).

[0048] 2-Naphthalene thiophenol d...

Embodiment 1

[0053] Precisely measure 0.1ml of 50μg / ml mesylate mixed stock solution, place it in a 5ml volumetric flask, add 1.0ml of 1.0mg / ml 2-naphthalene thiol derivatization solution and 0.10mol / L NaOH solution in turn 0.5ml, diluted 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 analysis.

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

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

Embodiment 2

[0057] Precisely measure 6 parts, each 0.10ml of the serial mesylate mixed stock solution, place them in 6 5ml volumetric flasks, add 1.0ml and 0.50mol / ml of 5.0mg / ml 2-naphthalene thiophenol derivatization solution 0.5ml of L NaOH solution, dilute to the mark with acetonitrile, shake well, prepare a solution of 0.1, 0.2, 0.4, 0.6, 0.8, 1.0 μg / ml of mesylate, respectively, react at 80 °C for 2 h, and let it cool until At room temperature, centrifuge at 10,000 rpm for 5 min, and take 20 μl of the supernatant and inject it into HPLC-UV analysis.

[0058] Take about 100 mg of imatinib mesylate, accurately weigh it, place it in a 10 ml measuring flask, dissolve it with water-acetonitrile solution (10:90, v / v) and dilute it to the mark. Precisely measure 0.5ml, put it in a 5ml measuring bottle, add 1.0ml of 5.0mg / ml 2-thionaphthalene derivatized solution and 0.5ml of 0.50mol / L NaOH solution, dilute with acetonitrile to the mark, shake well, put it in The reaction was carried out a...

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Abstract

The invention belongs to the technical fields of analysis and detection of drugs and particularly relates to a method for measuring methanesulfonate by virtue of a derivatization HPLC-UV method. According to the method, methanesulfonate is derivatized by virtue of a 2-thionaphthol derivatization agent to generate a derivated product with absorptivity in an ultraviolet region of 252nm-253nm, and the derivated product of methanesulfonate is measured in the ultraviolet region of 252nm-253nm by virtue of an HPLC reversed phase partition chromatography, thereby realizing the qualitative and quantitative determination of methanesulfonate in a raw material drug containing methanesulfonic acid. In the measurement process of the method, the analysis is not interfered by imatinib mesylate and otherimpurities in imatinib mesylate, so that the specificity of the method is good; the detection limit of the method is 0.03microg / ml, the quantitation limit is 0.10microg / ml, and the linear relation isgood; the average recovery rate is 87.5%-102.1%, and the obvious matrix interference avoided; and the derivated product has good stability within 6 hours.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and detection, in particular to a method for determining mesylate by a derivatized HPLC-UV method. Background technique [0002] Potential genotoxic impurities are strong mutagenic and carcinogenic agents that can cause DNA mutations, chromosomal breaks or DNA recombination, and may also lead to tumorigenesis in humans. In recent years, with the gradual improvement of genotoxic impurity regulations, the US Food and Drug Administration (FDA) and European Medicines Agency (EMEA) and other departments have higher and higher regulatory requirements for genotoxic impurities. Improper control of genotoxic impurities in drugs may lead to clinical hidden dangers and also affect the time to market of new drugs. Therefore, it is very important to control potential genotoxic impurities in the drug production process. [0003] Mesylates, a common class of potentially genotoxic impurities, have received...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 徐洁
Owner ZIBO VOCATIONAL INST
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