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A kind of formaldehyde derivative test method

A test method and technology of derivatization reagents, applied in the field of formaldehyde derivatization test, can solve the problems of time-consuming, complicated derivatization reaction process, easy to generate interference, etc., and achieve the effect of simplifying the test method, improving sensitivity and simple reaction

Active Publication Date: 2022-01-14
长沙晨辰医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] For the detection of formaldehyde whose detection limit is required to be less than 1.5ppm, the liquid-phase DNPH method is prone to interference, and the derivatization reaction process is complicated and time-consuming

Method used

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  • A kind of formaldehyde derivative test method
  • A kind of formaldehyde derivative test method
  • A kind of formaldehyde derivative test method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Formaldehyde residue method verification in embodiment 1 rifampicin

[0057] 1. Instruments, reagents, reference substances and test substances

[0058] Instrument: one hundred thousandth analytical balance, gas chromatography-mass spectrometry (Agilent 7890A-5975C);

[0059] Solvents: formaldehyde solution (38.25%), methylamine hydrochloride (98%), dimethylsulfoxide (DMSO, HPLC), dicyclohexylcarbodiimide (DCC).

[0060] 2. Solution preparation

[0061] Derivative reagent: take 500mg DCC and 100mg methylamine hydrochloride, weigh them accurately, put them in a 100ml volumetric flask, dilute to the mark with DMSO, and shake well;

[0062] Blank solution: pipette 2.0ml of derivatization reagent and 2.0ml of DMSO respectively, put them in a 10ml digestion tube, wait until the temperature of the digestion instrument rises to 60°C, put the digestion tube into the digestion instrument for derivatization for 30min, after the digestion is completed, cool to room temperature, ...

Embodiment 2

[0190] Determination of formaldehyde residual content in the duloxetine hydrochloride starting material of embodiment 2

[0191] 1. Instruments, reagents, reference substances and test substances

[0192] Instruments: 1 / 100,000 analytical balance, gas phase-mass spectrometer;

[0193] Solvent: formaldehyde solution (38.25%), methylamine hydrochloride (HPLC), dimethyl sulfoxide (HPLC), strongly acidic cationic resin (AR);

[0194] 2. Solution preparation

[0195] Derivative reagent: take 500mg DCC and 100mg methylamine hydrochloride, weigh them accurately, put them in a 100ml volumetric flask, dilute to the mark with DMSO, and shake well;

[0196] Blank solution: Pipette 2.0ml of derivatization reagent and 2.0ml of DMSO into a 10ml digestion tank. After the temperature of the digestion instrument rises to 60°C, place the digestion tube in the digestion instrument for 30 minutes of derivatization. After the digestion is completed and cooled to room temperature, transfer 2.0ml...

Embodiment 3

[0216] Determination of residual formaldehyde content in febuxostat in embodiment 3

[0217] 1. Instruments, reagents, reference substances and test substances

[0218] Instrument: 1 / 100,000 analytical balance, coupled with gas chromatography-mass spectrometry;

[0219] Reagents: acetonitrile (HPLC), ethanol (HPLC), strongly acidic cationic resin (AR);

[0220] Reference substance: formaldehyde (38.25%);

[0221] Sample: febuxostat.

[0222] 2. Solution preparation

[0223] Derivative reagent: take 500mg DCC and 100mg methylamine hydrochloride, weigh them accurately, put them in a 100ml volumetric flask, dilute to the mark with DMSO, and shake well;

[0224] Blank solution: Pipette 2.0ml of derivatization reagent and 2.0ml of DMSO into a 10ml digestion tank. After the temperature of the digestion instrument rises to 60°C, place the digestion tube in the digestion instrument for 30 minutes of derivatization. After the digestion is completed and cooled to room temperature, tra...

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Abstract

The invention provides a method for testing formaldehyde derivatization, which comprises the following steps: preparing a reference substance solution and a test solution; The reaction is carried out under microwave-assisted conditions; the test solution is prepared by the following steps: the derivatization reagent is mixed with the test product liquid, and the reaction is carried out under microwave-assisted conditions; wherein, the derivatization reagent is dissolved in DCC and methylamine Obtained in an organic solvent; adopt gas chromatography-mass spectrometry, analyze the reference substance solution and the test sample, record the chromatogram, combine the formaldehyde content in the reference substance solution, and calculate the N-methyl group according to the peak area external standard method The content of methyleneamine, thereby obtain the content of formaldehyde in the test sample. By adopting the technical solution of the invention, the derivative product has strong response in GC / MS, simplifies the test method of formaldehyde, and improves the sensitivity of detecting formaldehyde.

Description

technical field [0001] The invention relates to the technical field of formaldehyde detection, in particular to a formaldehyde derivative test method. Background technique [0002] Formaldehyde is a colorless gas with a pungent smell, and it is also a toxic substance with a relatively high content in today's home decoration. Different degrees of formaldehyde pollution and different people will cause different degrees of harm, from mild asthma, cough, cold, etc., to various diseases caused by severe immunity decline. At present, the content of formaldehyde is generally known through indoor formaldehyde detection, and then treated to reduce the content of harmful substances in the indoor air, thereby reducing the harm of formaldehyde to the human body. There are many commonly used formaldehyde detection methods, but each has its advantages and disadvantages. The specific analysis is as follows: [0003] (1) Colorimetric method and spectrophotometer method [0004] The detec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/067
Inventor 熊学武高旭杨强温贤明
Owner 长沙晨辰医药科技有限公司