Method for detecting benzopyrene in smoked sturgeons

A detection method and technology of benzopyrene, applied in the detection field of benzopyrene, can solve the problems of inability to detect products by detection equipment, detection interference, poor detection effect, etc., and achieve excellent multi-path effect and radial and axial diffusion effect, Good detection specificity and detection effect, good extraction efficiency and recovery effect

Active Publication Date: 2018-08-10
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current extraction method for 3,4-benzopyrene cannot remove the small molecular impurities in smoked aquatic products, and these impurities will interfere with the detection of 3,4-benzopyrene, resulting in detection equipment The product cannot be tested normally, and the detection effect is poor
In addition, the existing detection methods for 3,4-benzopyrene still have problems such as low specificity and low sensitivity, which are difficult to meet people's requirements for food safety.

Method used

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  • Method for detecting benzopyrene in smoked sturgeons
  • Method for detecting benzopyrene in smoked sturgeons
  • Method for detecting benzopyrene in smoked sturgeons

Examples

Experimental program
Comparison scheme
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preparation example Construction

[0048] The 3,4-BaP molecularly imprinted polymer is Ti4 + -IMAC monodisperse microspheres, the preparation process is as follows figure 1 Shown, its preparation method comprises the following steps:

[0049] ①Dissolve 1.14mL of surfactant Triton-X100 and 1.25g of polyvinylpyrrolidone in 64mL of ethanol to obtain product G;

[0050] ② Dissolve 0.58g of azobisisobutyronitrile (AIBN) in 16mL of styrene monomer, then slowly add product G, then heat the mixture to 70°C and stir for 24 hours to make the mixture gradually change from transparent to milky white. Get H product;

[0051] ③Centrifuge product H at 10,000 g for 5 minutes at room temperature, then collect the precipitate and wash it with 20 mL of ethanol for 3 times to obtain product I (polystyrene monodisperse microspheres);

[0052] ④ configure 165mL of polyvinyl alcohol (PVA) and sodium dodecyl cyclamate (SDS) mixed solution (PVA & SDS aqueous solution), to obtain J product, wherein the concentration of polyvinyl alco...

experiment example 1

[0066] Experimental example 1: 3,4-BaP standard with a purity of ≥99% was prepared in methanol as a solvent to form a 10 μg / mL 3,4-BaP standard stock solution, which was then prepared into 6 concentrations of 3,4-BaP with a blank matrix solution Standard working solution, with the peak area (y) of 3,4-BaP chromatogram as the ordinate, the mass concentration (x, μg / kg) as the abscissa to draw the standard curve, draw the linear regression equation y=3726x+1233.5, linear The range is 5-1000 μg / kg, and the correlation coefficient is 0.9998. At the same time, the standard addition method was used for determination, and the method detection limit (LoD) and quantification limit (LoQ) of the analyte were determined according to the signal-to-noise ratio (S / N) of 3 and 10 times, respectively. The results are shown in Table 2. The linearity of 3,4-BaP is good, and the detection limit and quantification limit are 0.98 and 3.16 μg / kg, respectively, meeting the needs of high-sensitivity d...

experiment example 2

[0071]Experimental Example 2: 30 batches of commercially available smoked sturgeon and 20 batches of smoked sturgeon developed by the research group were tested using the detection method established by the present invention, and the results were analyzed mathematically and statistically. It was found that among the 50 batches of smoked sturgeon, a total of 12 samples were detected positive for 3,4-BaP, with a detection rate of 24%, except for one batch of smoked sturgeon with a 3,4-BaP content of 21.9 μg / kg, although there were 3,4-BaP positive signals in the remaining batches of smoked sturgeon, they were lower than the limit of quantification and met the international limit standard. The results show that the present invention is suitable for the detection of 3,4-BaP in smoked sturgeon, and the relevant data can provide relevant basis and reference for functional departments, and then provide protection for consumers' food safety.

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Abstract

The invention discloses a method for detecting benzopyrene in smoked sturgeons. The method comprises the following steps: adding minced fillet of smoked sturgeons into an acetonitrile-acetone mixed extracting solution, and oscillating to be uniform; adding excessive sodium chloride for centrifuging, centrifuging the supernatant, evaporating to dryness, and re-dissolving with 2mL of normal hexane to obtain an extracting solution; suspending Ti4<+>-IMAC mono-dispersion microspheres in dichloromethane to serve as packing to be filled in an empty solid-phase extraction column, pressing to make a molecular imprinting solid-phase extraction column, activating the solid-phase extraction column, and enabling the extracting solution to slowly flow through the column; leaching, draining, eluting andtaking the collection fluid, performing nitrogen blowing, volume fixing and passing through a filter membrane so as to obtain a to-be-detected item, and finally detecting the to-be-detected item by virtue of liquid chromatography-tandem mass spectrometry. The method disclosed by the invention has the characteristics of being high in specificity, high in detection accuracy and excellent in detection effect.

Description

technical field [0001] The invention relates to a method for detecting benzopyrene, in particular to a method for detecting benzopyrene in smoked sturgeon. Background technique [0002] Sturgeon is the largest freshwater fish in the world. It has great processing potential because of its delicious, fatty and nutritious meat. Because the smoked sturgeon meat has a unique color and aroma, most current manufacturers use the smoking method. Process the sturgeon. However, when the sturgeon is smoked or roasted under the influence of high temperature, a large amount of benzopyrene will be formed through cracking and thermal polymerization reactions, and 3,4-benzopyrene (3,4-BaP) is a representative thickener. Aromatic hydrocarbons are highly carcinogenic and can damage DNA, cause cancerous cells and cause damage to internal organs and the nervous system. Therefore, in order to ensure food safety for consumers, functional departments need to accurately detect benzopyrene in smoke...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 沈清林亚楠陈康戴志远
Owner ZHEJIANG GONGSHANG UNIVERSITY
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