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Method for detecting bisphenol compounds

A technology of phenolic compounds and bisphenols, which is applied in the field of analytical chemistry, can solve the problems of unsuitable residue identification, high mobile phase viscosity, and consumption of organic reagents, and achieve the effects of high accuracy, high separation efficiency, and convenient operation

Active Publication Date: 2022-03-01
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The currently reported detection methods for bisphenols in food contact materials include enzyme-linked immunosorbent assay, high performance liquid chromatography ultraviolet detection method, high performance liquid chromatography fluorescence detection method, etc. However, these traditional methods have their disadvantages to a certain extent. disadvantages
Enzyme-linked immunosorbent assay is a special reaction between antigen and antibody, which may lead to false positive results. It is only suitable for rapid detection and not suitable for residue identification
The high viscosity of the mobile phase in high performance liquid chromatography results in reduced flow rates and thus longer analysis times
With the development of mass spectrometry, gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry are widely used in the field of food safety. However, gas chromatography-mass spectrometry requires a complex derivatization process, which is tedious and time-consuming; Reagents, causing environmental pollution

Method used

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  • Method for detecting bisphenol compounds
  • Method for detecting bisphenol compounds
  • Method for detecting bisphenol compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The rapid quantitative detection of bisphenols in polycarbonate provided by the present embodiment comprises the following steps:

[0049] 1. Sample processing and testing

[0050] Grind the polycarbonate sample into small particles with a refrigerated grinder, add dichloromethane to the sample and sonicate until it is completely dissolved, slowly add methanol dropwise, centrifuge the cloudy solution, take the supernatant liquid nitrogen and blow it nearly dry, and reconstitute it with n-hexane and isopropanol After vortexing, the membrane was filtered, and the filtered liquid was injected into UPCC-MS / MS for detection and analysis.

[0051] 2. Make a standard curve

[0052] Put a variety of standard products of bisphenol compounds in volumetric flasks, add methanol to dissolve and constant volume, and prepare a single-standard stock solution; take the same volume of each bisphenol compound single-standard stock solution for mixing, add n-hexane Diluted with isopropan...

Embodiment 2

[0060] In order to improve the comprehensiveness and accuracy of the detection method for bisphenol compounds, this embodiment compared and analyzed the different experimental conditions of UPCC-MS / MS, optimized the detection method provided in this embodiment, and facilitated the comprehensive detection of the above-mentioned 17 bisphenol compounds.

[0061] In the UPCC-MS / MS method of this embodiment, Waters ACQUITY UPC is used respectively 2 BEH, Torus 1-AA, Torus 2-PIC, Torus DEA and Torus DIOL chromatographic columns (100mm×3mm, 1.7μm) were used for detection, and the retention and separation of the 17 target objects by the above five chromatographic columns were compared, and the same The mixed standard solution of concentration, adopts above-mentioned five kinds of chromatographic columns to carry out ultra-efficient convergence chromatographic experiment respectively, the chromatographic peak separation situation of 17 kinds of bisphenols shown in embodiment 1 is as fo...

Embodiment 3

[0067]Using the optimized rapid quantitative detection method for bisphenol compounds in polycarbonate provided in Example 2, the reliability of the detection method provided in this example was verified.

[0068] Perform pretreatment on the sample, accurately weigh 1g of polycarbonate in a stoppered glass bottle, add 14mL of dichloromethane as the extraction solvent, sonicate for 20min until it is completely dissolved, add 6mL of methanol dropwise, centrifuge the cloudy solution at 4000rpm for 5min, and take Blow 1mL of the supernatant to dryness with liquid nitrogen, reconstitute with 1mL of n-hexane-isopropanol (v / v, 8:2), vortex for 30s, pass through a 0.22μm filter membrane, and inject the filtered liquid into UPCC- Detection and analysis in MS / MS.

[0069] To make a standard curve, first prepare a single-standard stock solution: Accurately weigh 10 mg of each bisphenol compound standard, add an appropriate amount of 10 mL of methanol to dissolve and constant volume, prep...

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Abstract

The invention discloses a method for detecting bisphenol compounds. The method includes: extracting the sample to obtain a test solution; and using an ultra-high performance convergence chromatography tandem mass spectrometry system to detect the test solution so as to perform qualitative and / or quantitative analysis on the bisphenol compound . The method uses an ultra-high performance convergence chromatography tandem mass spectrometry system to detect bisphenol compounds. The ultra-high performance convergence chromatography has high separation ability and high sensitivity of mass spectrometry identification ability, and is suitable for the separation and identification of various bisphenol compounds in polycarbonate. Identification, high separation efficiency, accurate quantification, convenient operation, and environmental protection.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting bisphenol compounds. Background technique [0002] Bisphenol A (BPA) is a functional monomer for synthesizing polycarbonate and epoxy resin. In the manufacturing process of plastic products, adding bisphenol A can improve the colorless, transparent, durable, lightweight and impact-resistant properties of plastic products. Polycarbonate is often used to make food cans, baby bottles, eyeglass lenses, medical devices, etc. However, bisphenol A monomer may remain in plastic packaging materials during the production process, and then migrate into food, causing harm to human health. Bisphenol A is an environmental endocrine disruptor, which may also cause diabetes, regenerative system disorders, cardiovascular and cerebrovascular and immune system diseases, and other endocrine-related diseases at low exposure doses. Bisphenol A migrating from baby feeding bo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张峰凌云张雨佳姚美伊姚桂红
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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