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Method for enriching and detecting phthalate ester compound in wine sample by ionic liquid-dispersive liquid-liquid microextraction

A technology of ester compounds and phthalic acid, which is applied in the field of enrichment and detection of phthalate compounds in wine samples by ionic liquid-dispersion liquid-liquid microextraction, can solve the problems of complex organic matrix and high ethanol content , to achieve the effect of simple operation, less usage, accurate and effective measurement

Inactive Publication Date: 2014-05-28
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the dispersion liquid-liquid microextraction method is generally only suitable for the detection of water samples. The ethanol content of wine samples is high, the organic matrix is ​​complex, and phthalates have good solubility in wine. Liquid microextraction technology has not yet solved the problems of extraction, enrichment, purification and detection of phthalates.

Method used

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  • Method for enriching and detecting phthalate ester compound in wine sample by ionic liquid-dispersive liquid-liquid microextraction
  • Method for enriching and detecting phthalate ester compound in wine sample by ionic liquid-dispersive liquid-liquid microextraction
  • Method for enriching and detecting phthalate ester compound in wine sample by ionic liquid-dispersive liquid-liquid microextraction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Accurately pipette 25.00mL (three spiked samples of each of the following three concentrations) liquor samples were added with concentrations of 0.01, 0.05 and 0.10mg / L six common phthalates (phthalates) Diethyl dicarboxylate (DEP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), dicyclohexyl phthalate (DCHP), diethyl phthalate diethylhexyl ester (DEHP) and dioctyl phthalate (DOP)) in a glass centrifuge tube, add After dissolving 5g of sodium chloride, add 50 μL of 1-n-octyl-3-methylimidazolium hexafluorophosphate ionic liquid as the extraction agent, without adding a dispersant, and perform ultrasonic extraction (ultrasonic dispersion, such as commercially available conventional 50-500W power Ultrasonic emulsification apparatus, etc.; or use ultrasonic power: 150-1500W, ultrasonic frequency: 20--40KHz, power supply: 220 / 380V50HZ ultrasonic conditions can achieve ultrasonic dispersion) 15min, dispersed to form a microemulsion; centrifuge at 4000rpm After 15 minut...

Embodiment 2

[0029] Accurately pipette 25.00mL red wine samples to add six common phthalate compounds (diethyl phthalate (DEP), diisobutyl phthalate) at concentrations of 0.1, 0.5 and 1.0 mg / L (DIBP), dibutyl phthalate (DBP), dicyclohexyl phthalate (DCHP), diethylhexyl phthalate (DEHP) and dioctyl phthalate (DOP) ) of the spiked wine sample (red wine sample 2 with no phthalates detected) in a glass centrifuge tube, add 3g of sodium sulfate to the centrifuge tube respectively, after dissolving, add 50μL of 1-n-butyl-3-methyl The imidazole hexafluorophosphate ionic liquid was used as the extraction agent, 0.5 mL of acetone was added as the dispersant, ultrasonically extracted for 20 min, and dispersed to form a microemulsion; after centrifugation at 10,000 rpm for 5 min, the extractant precipitated at the bottom of the test tube. The volume of the precipitated phase was measured with a 100 μL microsyringe and transferred to a chromatography vial for liquid chromatography analysis.

[0030] ...

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Abstract

The invention relates to a method for enriching and detecting a phthalate ester compound in a wine sample by ionic liquid-dispersive liquid-liquid microextraction. According to the method, the phthalate ester compound in the wine sample is enriched by ionic liquid-dispersive liquid-liquid microextraction, and then trace amounts of a phthalate ester plasticiser in the wine sample are detected by headspace-gas chromatography-mass spectrometry or liquid chromatography. The method is characterized in that extraction, enrichment and purification of trace amounts of a phthalate ester plasticiser in a common wine sample are integrated; the content of the trace amounts of the phthalate ester plasticiser in the wine sample can be measured accurately and effectively; the method can be used in quality control of a wine sample; and the method is rapid and reliable and is simple to operate.

Description

technical field [0001] The invention relates to a method for enriching and detecting phthalate compounds in wine samples by an ionic liquid-dispersion liquid-liquid microextraction method. Specifically, the ionic liquid-dispersed liquid-liquid microextraction method was used to enrich the phthalates in the wine samples, and then the headspace-gas chromatography-mass spectrometry or liquid chromatography was used to detect trace phthalates in the wine samples. Dicarboxylate plasticizers. Background technique [0002] Phthalic acid ester compounds (Phthalic acidester, PAEs), also known as phthalic acid ester compounds, its chemical structure is generally composed of a rigid planar aromatic hydrocarbon and two plastic nonlinear aliphatic side chains (see the general structural formula (I) below shown). Mainly include: dimethyl phthalate (DMP), diethyl phthalate (DEP), dicyclohexyl phthalate (DCHP), dinonyl phthalate (DINP), phthalate Nonyl dicarboxylate (DNP), n-octyl phthal...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 沈昊宇朱奇程勇杰陈君良周阿蒙王哲君胡美琴
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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