A rapid quantitative detection method for bisphenol compounds in dairy products

A quantitative detection method and technology of bisphenols, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of prone to false positives, high pretreatment requirements, time-consuming and labor-intensive, etc., to achieve improved sensitivity and strong ability to precipitate proteins , identify the exact effect

Inactive Publication Date: 2018-01-16
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The GC-MS method (gas chromatography mass spectrometry) has certain limitations for the simultaneous analysis of such compounds, because bisphenols and epoxy derivatives have high melting points, and generally require post-column or pre-column derivatization methods, which are cumbersome to operate
All bisphenol compounds contain two or more benzene rings in their structure, and there are electron-donating groups such as hydroxyl groups on the para-position of the benzene rings, which have fluorescence characteristics, so HPLC-FLD (high performance liquid chromatography fluorescence detection method) can be used ) detection, but the liquid phase detection is only qualitative by retention time, prone to false positives, high requirements for pre-treatment, time-consuming and labor-intensive

Method used

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  • A rapid quantitative detection method for bisphenol compounds in dairy products
  • A rapid quantitative detection method for bisphenol compounds in dairy products
  • A rapid quantitative detection method for bisphenol compounds in dairy products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The rapid quantitative detection method for bisphenols in dairy products provided in this example comprises the following steps:

[0034] Sample Processing and Testing

[0035] Put the dairy product to be tested in a stoppered colorimetric tube, add extraction solvent, magnesium sulfate and sodium acetate, vortex and let it stand, take the supernatant and transfer it to another colorimetric tube, add magnesium sulfate and N- Purify with propylethylenediamine and C18, vortex and let it stand, take the supernatant liquid nitrogen and blow it nearly dry, and redissolve it with methanol and water, filter the membrane after vortex, take the filtered liquid and inject it into HPLC-MS Detection and analysis on / MS;

[0036] Make standard curve

[0037] Put a variety of bisphenol compound standard products 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 sta...

Embodiment 2

[0045] In order to improve the detection comprehensiveness and accuracy of the detection method provided in this embodiment, this embodiment carried out comparative analysis on different sample processing methods, and carried out comparative analysis on different experimental conditions of HPLC-MS / MS, and optimized this method. The detection method provided in the examples facilitates the comprehensive detection of the above-mentioned 21 kinds of bisphenol compounds.

[0046] In the HPLC-MS / MS method of this example, the chromatographic column can be an Agilent ZORBAX SB C18 column (2.1×50mm.i.d., 1.8μm) or an ACOUITY UPLC BEH C18 column (2.1×50mm.i.d., 1.7μm), for further The experimental conditions were optimized, and the retention and separation of 21 target substances by the two chromatographic columns were compared. The mixed standard solutions of the same concentration were respectively taken, and the above two chromatographic columns were used for ultra-high performance ...

Embodiment 3

[0060]Combined with the rapid quantitative detection method for bisphenol compounds in dairy products provided in Example 2, this example provides a preferred implementation of the rapid quantitative detection method for bisphenol compounds in dairy products, taking milk as an example to verify this embodiment The reliability of the provided detection method.

[0061] Pre-treat the sample, accurately weigh 5g of milk into a 50mL stoppered colorimetric tube, add 15mL of 1% acetic acid acetonitrile as the extraction solvent, add 4gMgSO 4 And 1.48g sodium acetate, vortex 1min. Stand still and transfer 10mL supernatant to another colorimetric tube, add 1gMgSO 4 , purified with 390mgPSA and 190mgC18, vortexed for 1min, took 6mL of supernatant liquid nitrogen and blown it nearly dry, reconstituted with 1.5mL of methanol-water (v / v, 50:50), vortexed for 30s and passed through a 0.22μm filter membrane, The filtered liquid was injected into HPLC-MS / MS for detection and analysis.

[...

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Abstract

The invention relates to a rapid quantitative detection method for bisphenol compounds in dairy products. The method comprises the following steps of a sample treatment and detection process and a standard curve making process, wherein the concentration of the bisphenol compounds in a to-be-tested sample is calculated through a standard curve of testing data obtained in the sample treatment and detection process. According to the detection method, an HPLC-MS / MS method is adopted, the high separating ability of a liquid chromatogram can the high-sensitivity authentication ability of a mass spectrum can be utilized at the same time to separate and authenticate multiple bisphenol compounds in the dairy products, separation efficiency is high, and authentication is accurate; 21 bisphenol compounds can be separated qualitatively and quantitatively, the extracted bisphenol compounds are high in recovery rate, and method can be effectively used for screening the bisphenol compounds in the dairy products.

Description

technical field [0001] The invention relates to the technical field of detection of bisphenol compounds in food, in particular to a rapid quantitative detection method of bisphenol compounds in dairy products. Background technique [0002] Bisphenol A (BPA) and bisphenol diglycidyl glycidyl ether (BADGE) are functional monomers of polycarbonate and epoxy resins, which can be used as antioxidants for phenolic resins, plastic polyesters, and PVC stabilizers Wait. In the manufacturing process of plastic products, adding bisphenol A (BPA) or bisphenol diglycidyl ether (BADGE) can make it have the characteristics of colorless, transparent, durable, lightweight and outstanding impact resistance. In the process of producing organosol resin, hydrochloric acid will be generated during thermal curing of the resin, which will lead to thermal degradation of the polymer. By adding BADGE substances, it can absorb the hydrochloric acid generated during thermal curing of the resin. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/88G01N2030/027G01N2030/146G01N2030/8809G01N2030/884
Inventor 张峰聂雪梅许秀丽程燕
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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