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Method for detecting impurities, namely meta-methylnitrobenzene and m-toluidine, in m-cresol simultaneously

A technology of m-methylaniline and nitrotoluene, which is applied in the field of analytical chemistry, can solve the problems of simultaneous detection without registration, inability to achieve micro-measurement, and low sensitivity, and achieve good linear relationship, high accuracy, and improved detection sensitivity. Effect

Inactive Publication Date: 2017-07-07
HYBIO PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the method described in the above-mentioned documents, nitrobenzene is used as internal standard, quantified with internal standard calibration curve method, and adopts direct sample injection method to measure, but this kind of method sensitivity is low, can't reach to contain m-nitrotoluene, m-cresol in detecting m-cresol Micro-determination of phenylaniline (the amount of m-nitrotoluene and m-methylaniline contained in m-cresol must not exceed 100ppm, so the detection method requires a highly sensitive detection line and limit of quantification)
In addition, this method has not been reported to detect m-nitrotoluene and m-methylaniline at the same time. Therefore, it provides a method with high accuracy and sensitivity that can detect these two impurities at the same time. It is of great significance to carry out quality control of the synthetic product m-cresol of the by-product to ensure that the quality of the product m-cresol meets the requirements

Method used

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  • Method for detecting impurities, namely meta-methylnitrobenzene and m-toluidine, in m-cresol simultaneously
  • Method for detecting impurities, namely meta-methylnitrobenzene and m-toluidine, in m-cresol simultaneously
  • Method for detecting impurities, namely meta-methylnitrobenzene and m-toluidine, in m-cresol simultaneously

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: the system adaptability test of the method of the present invention

[0038] 1. Reagent preparation

[0039] Preparation of reference substance mother liquor: Weigh 100mg of m-nitrotoluene and 100mg of m-methylaniline respectively, put them in a 100ml measuring bottle, add dimethyl sulfoxide to dilute to the mark, accurately measure 2ml, put them in a 20mL measuring bottle, add dimethyl Dilute with sulfoxide-methanol-DMF (60:35:5) mixed solvent to the mark, shake well, and obtain.

[0040] Preparation of reference substance: Accurately measure 1ml of reference substance mother solution, add dimethyl sulfoxide-methanol-DMF (60:35:5) mixed solvent to 10ml, shake well, and obtain.

[0041] System suitability solution: Accurately weigh 1000mg m-cresol, put it in a 10ml measuring bottle, add dimethyl sulfoxide-methanol-DMF (60:35:5) to dissolve in an appropriate amount, add 1ml reference substance mother solution, add dimethylsulfoxide Sulfoxide-methanol-DMF ...

Embodiment 2

[0045] Embodiment 2: the sensitivity detection test of the method of the present invention

[0046] 1. Reagent preparation

[0047] Preparation of the detection limit solution: measure 0.5ml of the system suitability solution described in Example 1, put it in a 20ml headspace bottle, add 4.5ml of mixed solvent, mix well, and seal it with a gland, to obtain the solution, the concentration is 10ppm.

[0048] Preparation of the limit of quantitation solution: measure 1.5ml of the system suitability solution described in Example 1 and place it in a 20ml headspace bottle, add 3.5ml of mixed solvent, mix well, and seal it with a gland, and the concentration is 30ppm.

[0049] 2. Detection method

[0050] According to the method in Example 1, 1 part of the detection limit solution and 6 parts of the quantification limit solution were taken, and continuous headspace sampling was carried out, and the peak area RSDs of the 6 parts of the quantification limit solution middle nitrotoluen...

Embodiment 3

[0051] Embodiment 3: The detection method of the present invention detects the linear relationship between m-nitrotoluene and m-methylaniline

[0052] Measure each reference substance mother liquor 0.3ml, 0.5ml, 0.75ml, 1.0ml, 1.25ml, 1.5ml respectively in embodiment 1 and place in 10ml volumetric flask, use dimethyl sulfoxide-methanol-DMF (60:35 :5) mixed solvent is diluted to scale, and the concentration of m-nitrotoluene and m-methylaniline is respectively 30ppm, 50ppm, 75ppm, 100ppm, 125ppm, 150ppm, as 30%, 50%, 75%, 100%, 125%, The mixed control linear solution at 150% level was analyzed according to the headspace method in Example 1, and the result: the m-nitrotoluene linear equation is y=2E+08x+34435, R 2 =0.9986; m-methylaniline linear equation is y=3E+08x+69282, R 2 =0.9983, show that this method measures m-nitrotoluene and m-toluene in the concentration range of 30ppm-150ppm, the linear relationship is good, see Figure 4 and Figure 5 .

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Abstract

The invention relates to the technical field of chemical industry and discloses a method for detecting impurities, namely meta-methylnitrobenzene and m-toluidine, in m-cresol simultaneously. The method comprises the following steps: diluting a to-be-detected m-cresol sample by using a mixed solvent of dimethyl sulfoxide, methanol and DMF to obtain a test sample solution, and taking the mixed solution of the meta-methylnitrobenzene and the m-toluidine as a control product solution; and performing sample introduction on the test sample solution and the control production solution by a headspace mode, performing gas chromatographic detection, and calculating the content of the impurities, namely the meta-methylnitrobenzene and the m-toluidine, in the m-cresol according to an external standard method and based on peak area. The sample is diluted by the mixed solvent of the dimethyl sulfoxide, the methanol and the DMF, sample instruction is conducted by the headspace mode, and chromatographic detection is conducted, so that the content of the minute amount of meta-methylnitrobenzene and m-toluidine in the product can be detected simultaneously and accurately, the detection sensitivity is greatly improved, and important practical value on production control of the product and quality control of the product is achieved.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for simultaneously detecting impurities m-nitrotoluene and m-methylaniline in m-cresol. Background technique [0002] m-Nitrotoluene, the English name is 3-Nitrotoluene, the molecular formula is C 7 h 7 NO 2 , the molecular weight is 137.14, the CAS number is 99-08-1, and it has the smell of nitrobenzene. M-nitrotoluene is often used in the preparation of m-toluidine and dyes, etc., which can irritate the eyes, respiratory tract and skin. Absorption into the body can cause methemoglobinemia, cyanosis, and severe poisoning can be fatal. [0003] m-methylaniline, the English name is m-Toluidine, the molecular formula is C 7 h 9 N. , CAS No. 108-44-1, colorless oily viscous liquid, will gradually turn brown when exposed to light or oxidized in air. M-methylaniline forms salt with acid, other properties are the same as aniline, and it is an intermediate o...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04G01N30/30G01N30/60G01N30/68
CPCG01N30/02G01N30/16G01N30/30G01N30/6078G01N30/68G01N2030/025G01N2030/167
Inventor 陈仰东李勇唐洋明陶安进袁建成
Owner HYBIO PHARMA
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