Fast detection method of benzo(a) pyrene in high-fat foods

A high-fat food and detection method technology, applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems that affect the accuracy of detection results, long cooling time, increase analysis time, etc., to achieve easy promotion and use, and reduce operation Step, cooldown reduction effect

Inactive Publication Date: 2010-11-10
XIAMEN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0007] The currently reported microwave-assisted extraction of benzo(a)pyrene in food samples generally uses a professional microwave digestion system, which is not only expensive and cumbersome to operate, but also requires a long cooling time after the extraction, which undoubtedly increases the The total extraction time; the analysis and detection method of the sample is usually the combination of high performance liquid chromatography and fluorescence spectroscopy and the combination of gas chromatography and flame ionization or mass spectrometry, so it is required that the sample needs to go through a purification step before analysis, which is Correspondingly, the total analysis time of the sample is increased, and since benzo(a)pyrene exists in trace amounts in food, it will cause a large loss after purification steps, which will affect the accuracy of the test results

Method used

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  • Fast detection method of benzo(a) pyrene in high-fat foods

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Effect test

Embodiment 1

[0034] Embodiment 1: Spicy shredded fish sample: after the shredded spicy fish is crushed, weigh 1.0 g of the sample in a 250 mL ground suction filter bottle, add 20 mL of normal hexane and 15 mL of 1mol / L potassium hydroxide-methanol solution, Cover the ground plug and put it into a household microwave oven together with a container containing 500mL of water. Set the output power of the household microwave oven to 140W. After extraction for 10 minutes, cool to room temperature, add 15mL ultrapure water to rinse, take out the upper layer of n-hexane, and rotate to evaporate To dryness, dilute to 5 mL with dichloromethane. Pipette 2mL of the solution to the conventional quartz fluorescence sample cell of the fluorescence photometer, and perform constant energy simultaneous fluorescence spectrum mapping. The instrument parameters are set as follows: constant energy difference Δ ν ‾ = 1400 cm ...

Embodiment 2

[0035] Embodiment 2: Similar to Embodiment 1, the difference is that the second-order derivation function is added to obtain as figure 2 The second derivative-constant energy simultaneous fluorescence spectra are shown. The "derivative baseline method" was used to read the signal intensity value of the sample at 397.5 nm, which was used as the derivative fluorescence intensity for quantitative calculation. Then add 4 μL of 1mg / L benzo(a)pyrene standard solution to the 2mL sample solution into the liquid pool, perform second derivative-constant energy simultaneous fluorescence spectrum mapping, and add the standard 4 times. The value reading method adopts the "derivative baseline method": such as figure 2 As shown, the connecting line of a and b in the figure is the baseline of the negative peak of the sample. At 397.5nm, read the signal intensity values ​​of the baseline of the negative peak of the sample and the negative peak of benzo(a)pyrene respectively, and calculate t...

Embodiment 3

[0036] Embodiment 3: sunflower oil sample: pipette 0.4g sunflower oil sample in 250mL ground-mouth suction filter bottle, add 20mL normal hexane and 25mL 1mol / L potassium hydroxide-methanol solution, cover ground-mouth plug Then put it into a household microwave oven together with a container containing 400mL of water, set the output power of the household microwave oven to 140W, extract for 10 minutes, cool to room temperature, add 15mL of ultrapure water to rinse, take out the upper layer of n-hexane, rotary evaporate to dryness, and use two Dilute to 5mL with methyl chloride. Pipette 2ml of the solution to the conventional quartz fluorescence sample cell of the fluorescence photometer, and carry out the surveying and mapping of the second derivative-constant energy simultaneous fluorescence spectrum. The instrument parameters are set as follows: constant energy difference Δ ν ‾ = 1400 cm ...

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Abstract

The invention provides a fast detection method of benzo(a) pyrene in high-fat foods, relating to a detection method of benzo(a) pyrene, which has simple and fast operation and low cost. The method comprises the following steps of: placing a sample of high-fat foods in a ground suction bottle, adding a potassium hydroxide-methyl alcohol solution and normal hexane, extracting together with water in a microwave oven, taking out, cooling, flushing, taking out a clear liquid of normal hexane after settlement and stratification, drying by rotary evaporation, and determining the volume by using dichloromethane to obtain a sample solution to be detected; mapping the constant energy synchronous fluorescence spectra of the sample solution to be detected by using a fluorescence spectrophotometer with derivative-constant energy synchronous scanning for the identification and the rough detection of benzo(a) pyrene; and adding a second derivation function, mapping second derivate-constant energy synchronous fluorescence spectra, reading data by adopting a derivate baseline method, and determining the quantity of benzo(a) pyrene in the sample solution to be detected by using a continuous standard addition method.

Description

technical field [0001] The invention relates to a method for detecting benzo(a)pyrene, in particular to a rapid fluorescence detection method for benzo(a)pyrene in high-fat food. Background technique [0002] Benzo(a)pyrene (benzo(a)pyrene) is the most important environmental and food pollutant among more than 200 kinds of polycyclic aromatic hydrocarbons that have been discovered, and it is also a strong carcinogen to humans and animals. Benzo(a)pyrene (is not only distributed in air, water, soil and other environmental media, but also widely exists in food. The way that benzo(a)pyrene harms humans is mainly food pollution, especially processed high-fat food The content of benzo(a)pyrene in (such as smoked food, baked food and fried food, etc.) is relatively high, and long-term consumption of food containing polycyclic aromatic hydrocarbons such as benzo(a)pyrene will pose a potential threat to human health. It can cause cancer to various organs of the body, such as lung, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 李耀群林丽容周娜李呐李秀英
Owner XIAMEN UNIV
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