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Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique

A technology for food contact materials and polycyclic aromatic hydrocarbons, which is applied in the detection field of polycyclic aromatic hydrocarbons, can solve the problems of baseline drift, long analysis time, poor qualitative and quantitative effect, etc., and achieves the effect of small interference, accurate analysis method and cheap instrument.

Inactive Publication Date: 2010-01-13
CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

my country's national standard is the gradient elution of methanol and water, while the foreign method is the gradient elution of acetonitrile and water. Although the above two methods can achieve the separation of polycyclic aromatic hydrocarbons, their disadvantage is that the analysis time is long (my country's national The standard is 60min), and there is a problem of baseline drift
In addition, polycyclic aromatic hydrocarbons can also be detected by thin layer chromatography fluorescence photometry, paper chromatography fluorescence photometry, fluorescence spectrophotometry or capillary column gas chromatography, but there are characteristics of low detection sensitivity and poor qualitative and quantitative effects.

Method used

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  • Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique
  • Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique
  • Method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Using toluene as a solvent, prepare a standard solution of polycyclic aromatic hydrocarbons, and perform gas chromatography-mass spectrometry GC-MS analysis and detection according to the above experimental conditions, wherein the gas chromatography-mass spectrometer inlet temperature is set to 280 ℃, and the interface temperature Set to 280°C; the carrier gas is helium, and the flow rate is 1 ml / min; the temperature of the column is controlled in a programmed temperature mode, starting from 90°C, rising to 120°C at a rate of 30°C / min, and holding for 1 minute; then Then the temperature was raised to 300°C at a rate of 15°C / min and held for 15 minutes; the ion source for mass spectrometry detection was an electron bombardment source (EI source), the ion source bombardment energy was 70eV, and the ion source temperature was set to 230°C; 1 µl.

[0026] Figure 1a is the chromatogram of the polycyclic aromatic hydrocarbon standard solution detected in Example 1 of the pre...

Embodiment 2

[0030] Accurately weigh 0.5000 g of the fresh-keeping box sample into a headspace bottle, add an appropriate amount of toluene, and place it in an ultrasonic water bath extractor. After ultrasonic extraction at 60 °C for 3 hours, the extract is taken for gas chromatography-mass spectrometry. Ten parallel samples were made for this sample, and the experimental numbers were A, B, C, D, E, F, G, H, I, and J. The analysis results were shown in Table 2, and the first parallel sample (test number A) was The measurement was repeated 5 times, and the analysis results are shown in Table 3. The analysis results found that only naphthalene was present in the fresh-keeping box sample, and other 15 kinds of polycyclic aromatic hydrocarbons were not detected ( figure 2As shown, the uncertainty analysis results are shown in Table 4. The detection and analysis results show that the fresh-keeping box contains 1.10 mg / kg of naphthalene, and the uncertainty is 8.0%.

[0031] Table 2 Test content...

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Abstract

The invention provides a method for detecting polycyclic aromatic hydrocarbon in food contact material by gas chromatogram-mass spectrometry coupling technique, comprising: Soxhlet extraction method or ultrasonic extraction method is used for extracting the detected food contact material; the extract sample is detected by a gas chromatogram-mass spectrometry coupling instrument; the temperature of a sample inlet of the instrument is set to be 240-320 DEG C, and the flow rate of carrier gas is set to be 0.5-2.0ml / min; a weakly polar chromatographic column is adopted, and the interface temperature is set to be 180-300 DEG C; the pretreated sample enters into the chromatographic column through the sample inlet of the instrument for temperature programming, and the temperature is raised to be 270-330 DEG C from 70-100 DEG C; after being separated by the chromatographic column, all the components in the sample are detected by mass spectrum. The method has the characteristics of low price of the detection instrument, safety, accurate and rapid analysis method and little interference as well as being suitable for standard analysis and detection which can lead all the components of the polycyclic aromatic hydrocarbon in the sample to be cracked in a mass spectrum ion source and optimize all the components of the cracked product, etc.

Description

technical field [0001] The invention relates to a method for detecting polycyclic aromatic hydrocarbons, in particular to a method for detecting polycyclic aromatic hydrocarbons in food contact materials by means of gas chromatography-mass spectrometry technology. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) refer to compounds composed of two or more benzene rings arranged in linear, angular or cluster shapes, including more than 150 compounds such as naphthalene, anthracene, phenanthrene, and pyrene. A class of chemical carcinogens and environmental pollutants that are ubiquitous in the environment. Polycyclic aromatic hydrocarbons are refractory to biodegradability and accumulation, and their most prominent features are carcinogenicity, teratogenicity and mutagenicity, and the carcinogenicity increases with the increase of the number of benzene rings. It has been confirmed that naphthalene, acenaphthene, acenaphthene, fluorene, phenanthrene, anthr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/72
Inventor 李向红刘永乐刘展谢定
Owner CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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