Method for rapidly extracting and purifying four kinds of polycyclic aromatic hydrocarbon compounds in edible oil, and detection application thereof

Abstract

The invention discloses a method for rapidly extracting and purifying four kinds of polycyclic aromatic hydrocarbon compounds in edible oil, and a detection application thereof. The method is characterized by comprising the following steps: (1) weighing an edible oil sample to be tested, adding an extracting solution and lipase in sequence, after constant temperature oscillating enzymolysis, adding potassium carbonate and ethanol or sodium carbonate and ethanol, and performing vortex uniform mixing; (2) then adding n-hexane and water, and after oscillating centrifugation, performing separationto obtain an upper layer organic phase and a lower layer aqueous phase; and (3) repeatedly extracting the lower layer aqueous phase once according to the method in step (2), mixing the upper layer organic phases obtained in the twice extraction, uniformly mixing the upper layer organic phases, performing rotary evaporation on the mixture at 40 DEG C until the mixture is dry, redissolving the mixture with acetonitrile, and filtering the solution with a filtering membrane for analysis. The detection application is to perform sample pretreatment according to the above method, and then perform liquid chromatography-fluorescence detection, and perform calculation according to a quantitative relationship between the concentration of 4 kinds of PAHs and instrument response values to obtain the contents of the 4 kinds of PAHs in the liquid to be tested. The method has the advantages that the extraction recovery rate is high, and the method is simple and fast, and high in sensitivity and accuracy.

Description

technical field [0001] The invention relates to a pretreatment and detection method of four kinds of polycyclic aromatic hydrocarbons in edible oil, in particular to a rapid extraction and purification method of four kinds of polycyclic aromatic hydrocarbons in edible oil and its detection application. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs), as a class of strong carcinogenic compounds, mainly come from edible oils that are repeatedly used or fried at high temperatures. Benzo[a]anthracene (BaA), benzo[b]fluoranthene ( BbF), benzo[k]fluoranthene (BkF) and benzo[a]pyrene (BaP) are four PAHs with strong toxicity, among which BaP is classified as a class 1 carcinogen by the International Agency for Research on Cancer, and the other three are classified as carcinogens. It is a class 2B carcinogen. Driven by huge profits, abnormal edible oils appear more and more frequently in people's lives, which poses a huge threat to people's health. The state se...

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Problems solved by technology

Among them, the solid-phase extraction column is retained on the adsorbent through hydrogen bond interaction. Although it can effectively remove the oily matrix, the operation process is cumbersome and time-consuming, and the reproducibility is poor; although the GPC method has the advantage of automation, it takes 3 hours per sample. The purification is completed in one hour, and a large amount of organic solvent is consumed, and the experimental cost is high

For example, Wu Chunying et al. established the Oasis HLB column purification method for benzo(a)pyrene in kitchen waste. In order to avoid oil elution, medium polar acetonitrile was used as the eluent; similarly, Wang Xi et al. used QuEChERS / Purification technology extracts and purifies polycyclic aromatic hydrocarbons in Lycium barbarum seed oil. Acetonitrile is used as the extraction solution, which cannot guarantee a high recovery rate for lipophilic compounds containing multiple ring structures.

Wang Lei and others established a gel chromatography purification method for benzopyrene in peanut oil. After purification by gel permeation chromatography, it was combined with alumina packed column to remove oil, which minimized the interference of oil matrix and ensured high recovery. rate (>95%), but this method consumes a lot of organic solvents, and the GPC purification process is cumbersome and time-consuming. As the amount of samples detected increases year by year, this method greatly limits the application of this method in daily inspections.

How to effectively extract lipophilic compounds from oils has always been a difficult challenge

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