Highly effective liquid phase chromatogram analyzing method of N-phenyl maleimide

A high-performance liquid chromatography, maleimide technology, applied in the direction of analysis of materials, material separation, measurement devices, etc., to achieve reliable analysis methods and simple quality control

Inactive Publication Date: 2007-08-08
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method for measuring N-PMI product and impurity aniline and maleic anhydride therein has not been reported yet

Method used

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  • Highly effective liquid phase chromatogram analyzing method of N-phenyl maleimide
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  • Highly effective liquid phase chromatogram analyzing method of N-phenyl maleimide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the selection of chromatographic conditions

[0033] 1.1 Selection of mobile phase

[0034] The mobile phase compositions with different volume ratios were compared, and the acetonitrile ratio was tested from high to low. The results showed that: when the acetonitrile ratio> 75%, the separation of the two impurity peaks is not good, and when the acetonitrile ratio> 80%, the two impurity peaks are difficult to separate , when the volume ratio of acetonitrile and water is 40:60, each component can achieve baseline separation, as shown in Figure 1.

[0035] 1.2 Selection of detection wavelength

[0036] Use a diode array detector to scan continuously at 200-400nm. It can be seen that N-PMI has a maximum absorption at 217nm, while aniline has a maximum absorption at 250nm, and maleic anhydride has a maximum absorption at 210nm. Taking into account the sensitivity of each component, select the detection The wavelength is 217nm.

[0037] 1.3 Sample concentrat...

Embodiment 2

[0039] Embodiment 2: the preparation of standard solution and sample solution

[0040] Accurately weigh 100.0 mg of N-PMI reference substance, put it in a 100 ml volumetric flask, dissolve it with 10 ml of acetonitrile, then dilute to the mark with mobile phase, shake well, and obtain a standard stock solution with a concentration of 1.0 mg / ml, and use it gradually diluted to the desired concentration.

[0041] Accurately weigh 50.0mg of aniline and maleic anhydride reference substances respectively, place them in a 100ml volumetric flask, dissolve them with 10ml of acetonitrile, then dilute to the mark with mobile phase, shake well, and obtain a standard stock solution with a concentration of 0.5mg / ml. When used, serially dilute to obtain the required concentration.

Embodiment 3

[0042] Embodiment 3: the making of standard curve

[0043] When the concentrations of aniline and maleic anhydride are 0.0005-0.1mg / ml and 0.0075-0.5mg / ml respectively, inject 5 μl of the sample, and plot the peak area against the concentration, as shown in Figure 3 and Figure 4. The regression equation is:

[0044] A 苯胺(area) =508+7492.5C 苯胺 , r=0.99988

[0045] A 马来酐(area) =50.69+7494.8C 马来酐 , r=0.99987

[0046] When the concentration of N-phenylmaleimide is 0.0001-0.5 mg / ml, inject 5 μl, plot the peak area against the concentration, see Figure 2, and the regression equation is:

[0047] A N-PMI(area) =992.7+1967.2logC N-PMI , r=0.99993

[0048] When the signal-to-noise ratio S / N=3, the lowest detection limits of N-PMI, aniline and maleic anhydride were 0.00005 mg / ml, 0.00025 mg / ml and 0.003 mg / ml, respectively.

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Abstract

The invention discloses an N-phenyl maleimide HPLC analysis method. The invention uses RP-HPLC method, and HPLC conditions are: chromatography column: C18, 5mum, 150X4.6mm (I.D), the volume ratio of the mobile phase: acetonitrile: water = 40-60:60-40, flow rate: 0.8ml / min, column temperature: 30 deg.C, detection wavelength: 217nm, sample volume: 3-5mul, diluting the determined content sample concentration 50 times, and determining N-PMI and impurity content. The HPLC analysis method of the invention can accurately determine N-PMI main content, and meanwhile, it can accurately determine impurity maleic anhydride and aniline content, providing a simple and reliable analysis method for quality control of N-PMI production process.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method of N-phenylmaleimide. Background technique [0002] N-phenylmaleimide (N-PMI for short) is an important organic chemical raw material. In the process of polymer processing, the added N-PMI can be embedded in the polymer chain to improve the internal rotation resistance of the chain and enhance The heat-resistant properties of polymers are used as heat-resistant modifiers for ABS resins, PVC resins, and polymethyl methacrylates, and can also be used as cross-linking agents for polypropylene and polyvinyl chloride; adhesives can be prepared, Improves the bond between metal and rubber. The level of N-PMI content directly affects the quality of the corresponding resin, so it is necessary to strictly control its content. With the continuous development of plastics, resin and other industries, the demand for N-PMI will continue to increase, and its determination method will a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 钱柯君蒋旭亮王中文顾月萍
Owner SHANGHAI CHEM REAGENT RES INST
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