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Solid-phase micro-extraction capsule and application of same in detection of phenol environmental estrogen in beverage

An environmental estrogen and extraction technology, applied in the field of solid-phase microextraction capsules, can solve the problems of failure to meet the measurement requirements, complex solid-phase extraction operations, limited enrichment multiples, etc., and achieve high-sensitivity effects

Active Publication Date: 2016-05-04
SHANDONG ANALYSIS & TEST CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation of solid-phase extraction is still relatively complicated. For liquid samples with extremely low analyte concentrations, the enrichment factor is limited, which may not meet the determination requirements.

Method used

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  • Solid-phase micro-extraction capsule and application of same in detection of phenol environmental estrogen in beverage
  • Solid-phase micro-extraction capsule and application of same in detection of phenol environmental estrogen in beverage
  • Solid-phase micro-extraction capsule and application of same in detection of phenol environmental estrogen in beverage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: the preparation of solid-phase microextraction capsule

[0035] 1. Synthesis of Silver-Containing Metal-Organic Nanotubes

[0036] 4,4'-bipyridine (0.2mmol), 1,3,5-benzenetricarboxylic acid (0.1mmol) were added to 7mL of silver nitrate solution, the pH of the solution was adjusted to 6, and transferred to a polytetrafluoroethylene reaction kettle for 160 The reaction was carried out at ℃ for 3 days, and then naturally cooled to room temperature. Alternately washed with ethanol and water, dried at 80°C, and finally obtained silver-containing metal-organic nanotubes, the scanning electron microscope image is as follows: figure 1 shown.

[0037] 2. Preparation of Solid Phase Microextraction Capsules

[0038] Add 5 mg of the above materials into 500 μL of methanol, and sonicate for 30 min. Take a hollow fiber membrane about 2 cm long, seal one end, and slowly inject the evenly dispersed metal-organic nanotube methanol solution by injection. Finally, the m...

Embodiment 2

[0039] Example 2: Condition optimization for improving the enrichment effect of solid-phase microextraction capsules

[0040] The capsule that embodiment 1 prepares carries out solid-phase microextraction operation and is:

[0041] Add 10mL of the sample to be tested into the 20mL sample bottle, and add the prepared solid phase microextraction capsules into it. Add the rotor and extract for a period of time under the stirring action of the magnetic stirrer to complete the extraction process. After the extraction was completed, the capsules were taken out, put into the liner tube, and 200 μL of analytical solvent was added for ultrasonic desorption. After the analysis process is completed, the desorbed solution is directly injected into the sample for analysis.

[0042] In order to improve the enrichment effect of solid-phase microextraction capsules, several important experimental conditions affecting the extraction effect, such as ionic strength, stirring rate, extraction t...

Embodiment 3

[0048] Example 3: Investigation of the detection limit, linear range and correlation coefficient of the method for detecting bisphenol A, 4-nonylphenol and 4-octylphenol based on solid-phase microextraction capsules and fast liquid chromatography-tandem mass spectrometry

[0049] 1. Chromatography and mass spectrometry conditions:

[0050] Chromatographic column: AgilentC18 chromatographic column (4.6mm×150mm, 5μm); mobile phase: methanol:water=90:10 (volume ratio); flow rate 0.2mL / min, column temperature 30°C, electrospray ion source; negative ion mode; capillary Voltage 3.1kv; ion source temperature 130°C; cone gas flow 50L / h, collision pressure 0.32kPa(He); the detection adopts multiple reaction monitoring (MRM) mode, see Table 1 for details.

[0051] Under optimized conditions, the analytical parameters of bisphenol A, 4-nonylphenol and 4-octylphenol are shown in Table 2. The linear range of these three target analytes is 5-500 μgL -1 , the correlation coefficient (R) wa...

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Abstract

The invention discloses a solid-phase micro-extraction capsule and application of the same in detection of phenol environmental estrogen in a beverage. A preparation method for the solid-phase micro-extraction capsule comprises the following steps: adding 4,4'-dipyridine and 1,2,3-benzenetricarbonic acid into a silver nitrate solution, carrying out a reaction at 150 to 170 DEG C for 2 to 4 d, and then successively carrying out cooling to room temperature, washing and drying so as to obtain a metal-organic nanotube material containing silver; and adding 0.5 to 1.5 mg of the prepared nanotube material into per 100 [mu]L of methanol, carrying out uniform dispersion, then injecting the obtained mixture into a hollow fiber film with a sealed end, then sealing the other end of the hollow fiber film and carrying out drying so as to obtain the solid-phase micro-extraction capsule. The invention also discloses a method for detecting phenol environmental estrogen in a beverage by using the solid-phase micro-extraction capsule. According to the invention, detection of multiple components of phenol environmental estrogen in the beverage is realized; and the method has the characteristics of rapidness, high efficiency, high sensitivity and the like and provides novel detection technology for quality safety monitoring of the beverage.

Description

technical field [0001] The invention relates to a solid-phase microextraction capsule and its application in detecting phenolic environmental estrogen in beverages, belonging to the technical field of food inspection. Background technique [0002] Bisphenol A is an important raw material for the production of polycarbonate plastics and epoxy resins. The products involved include cosmetics, packaging materials, etc., and can also be used to produce fine chemical products such as plasticizers and flame retardants. As endocrine disruptors, nonylphenol and octylphenol can enter the human body through the food chain and accumulate in the human body, which will have a positive impact on the growth and reproduction of human cancer cells. All three are listed as priority hazardous pollutants by the European Union , is a typical phenolic environmental estrogen. Since January 17, 2005, the European Union Directive 2003 / 53 / EC has imposed corresponding restrictions on the use, circulat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/28B01J20/30G01N30/06G01N30/08
CPCB01J20/28014B01J20/281B01J2220/80G01N30/06G01N30/08G01N2030/062
Inventor 赵汝松李秋琳王珊珊王晓利王霞
Owner SHANDONG ANALYSIS & TEST CENT
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