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Dispersive solid-phase extraction-gas chromatography-mass spectrometry method for determining residual quantity of o-phenylphenol in fruit juice

A technology of o-phenylphenol and disperse solid phase, which is applied in the field of disperse solid phase extraction-gas chromatography, can solve the problems of insufficient development of o-phenylphenol residue detection methods, and achieve the effect of saving adsorption time

Active Publication Date: 2021-08-31
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is insufficient development of detection methods for o-phenylphenol residues in fruit juice beverages, which are consumed in large amounts and require lower limits. It is urgent to develop a rapid detection method suitable for o-phenylphenol residues in fruit juice beverages

Method used

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  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry method for determining residual quantity of o-phenylphenol in fruit juice
  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry method for determining residual quantity of o-phenylphenol in fruit juice
  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry method for determining residual quantity of o-phenylphenol in fruit juice

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Effect test

Embodiment 1

[0075] The present embodiment 1 adopts orange juice as the sample matrix to carry out the standard recovery experiment to verify the feasibility of the method of the present invention, according to the following steps:

[0076] After the orange juice sample is filtered through 80-mesh filter paper, add 10 mL of the orange juice sample and 10 mL of deionized water to a 50 mL centrifuge tube with stopper to adjust the pH value to 7.0; add 0.50 g of p-toluenesulfonate to the centrifuge tube For acid radical-magnesium aluminum hydrotalcite adsorbent, vortex mix at 2500rpm for 10min, centrifuge at 4500rpm for 3min, discard the supernatant; add 2ml sulfuric acid aqueous solution to the centrifuge tube, vortex for 30s, then add 1.0g anhydrous sodium sulfate and 2.00ml of extractant, vortex for 15min, centrifuge, take the supernatant to another 10mL centrifuge tube, add 0.1g of anhydrous sodium sulfate-sodium bicarbonate mixture to it, vortex for 1min, filter, and wait for sample injec...

Embodiment 2

[0079] The present embodiment 2 adopts peach juice as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, according to the following steps:

[0080] After the peach juice sample is filtered through 80-mesh filter paper, add 10 mL of the peach juice sample and 10 mL of deionized water to a 50 mL centrifuge tube with stopper to adjust the pH value to 7.0; add 0.50 g to the centrifuge tube The p-toluenesulfonate-magnesium aluminum hydrotalcite adsorbent, vortexed at 2500rpm for 10min, centrifuged at 4500rpm for 3min, discarded the supernatant; added 2ml of sulfuric acid aqueous solution to the centrifuge tube, vortexed for 30s, and then added 1.0g Anhydrous sodium sulfate and 2.00ml extractant, vortex for 15min, centrifuge, take the supernatant to another 10mL centrifuge tube, add 0.1g of anhydrous sodium sulfate-sodium bicarbonate mixture, vortex for 1min, filter , pending analysis.

[0081] ...

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Abstract

The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a dispersive solid-phase extraction-gas chromatography-mass spectrometry method for determining the residual quantity of o-phenylphenol in fruit juice. The method comprises the following steps: adjusting the pH value of filtered fruit juice, adsorbing a target compound in the fruit juice by using a novel p-toluene sulfonate radical-magnesium aluminum type hydrotalcite adsorbent, dissolving the adsorbent by using an acid to realize complete elution of the target compound, performing efficient extraction on the compound by using a small dose of organic solvent, and performing rapid analysis and determination by using a gas chromatography-mass spectrometry method. According to the invention, the novel adsorbent adopted by the method realizes rapid and efficient adsorption of a target object by adopting a dispersive solid-phase extraction mode; complete desorption of a target object can be realized by using an acid-dissolved adsorbent; and only a small amount of organic solvent is suitable for extraction, so that the method has remarkable safety, environment-friendly and economic advantages.

Description

technical field [0001] The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a dispersive solid-phase extraction-gas chromatography method for determining the residual o-phenylphenol in fruit juice. Background technique [0002] O-phenylphenol (o-phenylphenol, OPP) is a commonly used preservative, which is often used as a preservative for fruits and vegetables, and there is a risk of seeping into the pulp during use. Studies have shown that this substance is toxic to the human liver, kidney, and nervous system, which has aroused people's great attention to its harm. The maximum limit value (MRL) set for o-phenylphenol residues in fruit juice in my country's mandatory national standards is 0.5mg / kg, the requirements are more stringent. [0003] Because o-phenylphenol is harmful to human health, people attach great importance to the detection of o-phenylphenol in leather, textiles, cosmetics and food contact materials, as well...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675G01N2030/047G01N2030/062
Inventor 丁立平
Owner 丁立平
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