Method for simultaneously detecting bisphenol A and phthalate esters based on ultraperformance convergence chromatography

An ultra-efficient phase combination and phthalic acid technology, applied in the field of chemical detection, can solve the problems of simultaneous detection of bisphenol A and multiple phthalate plasticizers, low detection efficiency, and long detection time, etc. problems, to achieve good application prospects, high detection efficiency, and short detection time

Active Publication Date: 2019-04-12
CHONGQING ACAD OF METROLOGY & QUALITY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the above-mentioned prior art, the purpose of the present invention is to provide a method for simultaneously detecting bisphenol A and phthalates in food based on ultra-high performance convergence chromatography, so as to solve the problem that existing detection methods cannot realize bisphenol A Simultaneous detection of multiple phthalate plasticizers, long detection time, low detection efficiency, etc.

Method used

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  • Method for simultaneously detecting bisphenol A and phthalate esters based on ultraperformance convergence chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Preparation of standard solution: Weigh bisphenol A and 18 kinds of phthalate standard products: BPA, BMPP, DIBP, DAP, DIPP, DPRP, DBP, DMP, DEHP, DHXP, DHP, DNOP, BBP , DNP, DPhP, DCHP, DBEP, DEEP and DMEP, use methanol to make standard solutions containing each standard substance, wherein the concentration range of each standard solution is 0.1~10.0 mg / L, and filter through a 0.22 μm organic filter membrane for use;

[0026] 2) Detection: The standard solution and the sample solution are gradiently eluted by ultra-high performance convergence chromatography, and the specification of the chromatographic column is ACQUITY UPC of 100mm×30 mm×1.7 μm 2 For CSH BEH, column temperature is 65°C, system back pressure is 1800psi, detection wavelength is 220 nm, mobile phase A is carbon dioxide and mobile phase B is acetonitrile; mobile phase elution gradient program is set as: 0~1min, mobile phase B The volume fraction of mobile phase B increased from 3% to 4.5%, and the flo...

Embodiment 2

[0029] A method for simultaneously detecting bisphenol A and phthalate plasticizers, comprising the steps of:

[0030] 1) Preparation of standard solution: Weigh bisphenol A and 18 kinds of phthalate standard products: BPA, BMPP, DIBP, DAP, DIPP, DPRP, DBP, DMP, DEHP, DHXP, DHP, DNOP, BBP , DNP, DPhP, DCHP, DBEP, DEEP and DMEP, use methanol to make standard solutions with gradient concentrations of each standard substance, wherein the concentration range of each standard solution is 0.1~10.0 mg / L, and after filtering with a 0.22 μm organic filter membrane, spare;

[0031] 2) Preparation of sample solution: cut the food contact material sample into small particles with a mass of ≤0.02 g, then accurately weigh 0.5 g of the sample to be tested, put it in a 25 mL stoppered glass test tube, add 10 mL of methanol, and Extract at low temperature for 30 min, then filter the extract with a 0.22 μm organic filter membrane, concentrate to nearly dryness, dilute to 1 mL with methanol, an...

Embodiment 3

[0035] 1) Preparation of standard solution: Weigh bisphenol A and 18 kinds of phthalate standard products: BPA, BMPP, DIBP, DAP, DIPP, DPRP, DBP, DMP, DEHP, DHXP, DHP, DNOP, BBP , DNP, DPhP, DCHP, DBEP, DEEP and DMEP, use methanol to make standard solutions with gradient concentrations of each standard substance, wherein the concentration range of each standard solution is 0.1~10.0 mg / L, and after filtering with a 0.22 μm organic filter membrane, spare;

[0036] 2) Preparation of the sample solution: cut the food contact material sample into small particles with a mass of ≤0.01g, then accurately weigh 1.0 g of the sample to be tested, put it in a 25 mL stoppered glass test tube, add 10 mL of methanol, and Extract at low temperature for 100 min, then filter the extract with a 0.22 μm organic filter membrane, concentrate to nearly dryness, dilute to 1 mL with methanol, and set aside;

[0037] 3) Detection: The standard solution and the sample solution are gradiently eluted by u...

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Abstract

The invention discloses a method for simultaneously detecting bisphenol A and 18 phthalate esters based on ultraperformance convergence chromatography. The method adopts ultraperformance convergence chromatography to perform gradient elution. The chromatographic column size is 150 mm x 30 mm, 1.7 [mu]m ACQUITY UPC2 CSHBEH. A mobile phase A is supercritical CO2 and a mobile phase B is an organic modifier. The column temperature is 50 to 70 DEG C. The flow rate is 0.8 to 1.5 ml / min. The system back pressure is 1700 to 2000 psi. The detection wavelength is 200 to 300 nm. The sample injection volume is 1 to 10 [mu]L. The invention can detect bisphenol A and 18 phthalate esters in 5.5 minutes. The invention has high sensitivity, good separation effect, short detection time and high detection efficiency, which can meet daily detection requirements of bisphenol A and phthalate esters plasticizers in food contact materials. The invention also provides theoretical guidance and technical supportfor the simultaneous detection of bisphenol A and 18 phthalate esters, and has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for simultaneously detecting bisphenol A and phthalates based on ultra-high performance convergence chromatography. Background technique [0002] In recent years, the migration of toxic and harmful substances in food contact materials is one of the main causes of food contamination. Bisphenol A and phthalates are environmental hormones and are widely used in food contact materials. A large number of studies have shown that both bisphenol A and phthalates can cause endocrine disorders, and are carcinogenic and reproductively toxic. In recent years, the European Union, the United States, China and other countries have restricted the use and migration of bisphenol A and some phthalates in food contact materials, while bisphenol A and phthalates in food contact materials New methods for the detection of esters have also become the focus of researchers. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 邱月李根容余秋玲龙梅陆嘉莉赵家雄
Owner CHONGQING ACAD OF METROLOGY & QUALITY INST
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