Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry

A technology of dimethyl fumarate and gas chromatography is applied in the field of detection of dimethyl fumarate in products, can solve the problems of high solvent consumption and high detection cost in liquid chromatography analysis, and achieves low cost of instruments and accurate analysis methods. , the effect of less interference

Inactive Publication Date: 2010-05-05
NINGBO PTS PROD TECH SERVICE
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] At present, there is a method for analyzing dimethyl fumarate by liquid chromatography. Although the liquid chromatography analysis method has strong separation and analysis capabilities, it can only quantitatively measure the content of each component in the product. For rapid , Accurate qualitative identification of components has certain limitations, and the use of liquid chromatography to analyze the solvent consumption is large, and the detection cost is high

Method used

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  • Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry
  • Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry
  • Method for measuring dimethyl fumarate in product by gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Accurately weigh 5.0mg of dimethyl fumarate, dissolve it with an appropriate amount of dehydrated ethyl acetate, transfer it to a 250ml volumetric flask, and dilute to the mark with dehydrated ethyl acetate, shake well, and stand still to obtain 20μg / ml DMF standard solution. The solution used for the test working curve of DMF was diluted step by step from the above 20 μg / ml standard solution, and prepared into a series of solutions of 0.1, 0.2, 0.5, 1.0, 2.0 μg / ml respectively, and carried out gas chromatography-mass spectrometry GC according to the above experimental conditions. -MS analysis and detection, in which the gas chromatography-mass spectrometry inlet temperature is set to 280 ° C, the interface temperature is set to 280 ° C; the carrier gas is high-purity helium, and the flow rate is 1 ml / min; the column temperature control adopts In the mode of programmed temperature rise, starting from 60°C, the temperature is raised to 100°C at a rate of 5°C / min; EI sou...

Embodiment 2

[0026] Cut the textile sample into a size of 4mm×4mm (ISO 4044:1998) with scissors, weigh about 0.5g, put it into a headspace bottle, add 5ml of dehydrated ethyl acetate extract (the sample needs to be fully shaken and wetted, and immersion in the extract), ultrasonically extract at 25°C for 30 minutes, and the working frequency of the ultrasonic instrument is 59KHZ. The ultrasonic extract was filtered with a 0.45 μm filter membrane, and the filtered extract was tested and analyzed by gas chromatography-mass spectrometry. The detection conditions of the gas chromatography-mass spectrometer were the same as in Example 1, and the external standard method was used for quantification. Three parallel samples were made on the textile sample, the test numbers were A, B, and C. The analysis results are shown in Table 1, and the first parallel sample (test number A) was measured 5 times. The analysis results are shown in Table 2. It can be seen from Table 1 that the relative standard d...

Embodiment 3

[0032]The standard solution in Example 1 was added to the prepared test solution with known negative (no target compound after testing), and the experiment was carried out according to the instrumental analysis and detection method in Example 1. Do 10 parallel measurements to the sample to get the average value, and calculate the standard recovery rate of the sample according to the actual addition amount and the actual measurement results. %, the relative standard deviation of parallel measurements was 2.14%.

[0033] Table 3 The recovery rate of the sample spiked

[0034] serial number

[0035] serial number

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Abstract

The invention discloses a method for measuring dimethyl fumarate in a product by gas chromatography-mass spectrometry. The method comprises the following steps of: pretreating a dimethyl fumarate product to be detected by using an ultrasonic extraction method; setting the temperature of a sample injection port of a gas chromatography-mass spectrometer to be 240-280 DEG C, a flow rate to be 0.8-1.5 ml/min and the temperature of a port to be 280-300 DEG C, and selecting a weak polar column for a chromatographic column; enabling a sample to enter the chromatographic column through the sample injection port, and carrying out temperature programming on the temperature of the chromatographic column to separate the components of the sample by the chromatographic column; and enabling the components separated by the chromatographic column to enter a mass spectrometric detection part through the port of the gas chromatography-mass spectrometer, wherein an electron impact ion source is adopted as the ion source of the mass spectrometric detection. The method for measuring the dimethyl fumarate in the product by the gas chromatography-mass spectrometry has low detection limit, good detection effect, little consumption of analysis solvent and low detection cost.

Description

technical field [0001] The invention relates to a detection method for dimethyl fumarate in products, in particular to a method for detecting dimethyl fumarate in products by gas chromatography-mass spectrometry. Background technique [0002] Dimethyl Fumarate (Dimethyl Fumarate, DMF for short) is a white powdery crystal with a slight ester fragrance. It can effectively inhibit and kill more than 30 kinds of molds, yeasts and bacteria. Therefore, it is widely used in industry, agriculture, food and other industries. For example, DMF is used for anti-mold of building materials, wood products and plastic products. It is also used in food and catering industry, medicinal materials, tobacco, textiles, film, leather and its products, paper. Anti-mildew, anti-moth and disinfection of coatings, dyes, adhesives, etc. [0003] However, studies have shown that DMF can enter the human body through the digestive tract, respiratory tract and skin, causing skin allergies, irritating the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/54
Inventor 刘展李向红陆斌李伟盛李建朱利平
Owner NINGBO PTS PROD TECH SERVICE
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