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Liquid chromatographic detection method of polycyclic aromatic hydrocarbons in edible oil

A technology of polycyclic aromatic hydrocarbons and liquid chromatography, which is applied in the field of food safety testing and can solve problems such as low recovery, no recovery, and poor retention

Inactive Publication Date: 2018-01-19
山东龙大粮油有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The biggest disadvantage of this method is that the SPE column has poor retention of highly polar compounds such as naphthalene, acenaphthene, fluorene, and phenanthrene, and the recovery rate is very low or even no recovery.

Method used

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  • Liquid chromatographic detection method of polycyclic aromatic hydrocarbons in edible oil
  • Liquid chromatographic detection method of polycyclic aromatic hydrocarbons in edible oil
  • Liquid chromatographic detection method of polycyclic aromatic hydrocarbons in edible oil

Examples

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Embodiment 1

[0056] Example 1, a liquid chromatography detection method for polycyclic aromatic hydrocarbons in edible oil. The edible oil in this example is first-grade soybean oil. The precision and accuracy of the verification method includes the following steps:

[0057] 1) Extraction: Weigh 2g samples each into six 50ml clean centrifuge tubes, add 0.1ml standard working solution to each centrifuge tube, add 2ml acetonitrile-saturated n-hexane to dissolve soybean oil, then add 20ml n-hexane-saturated acetonitrile , shake for 3 minutes, freeze at 0°C for 5 minutes and centrifuge, transfer the acetonitrile layer to a 100ml eggplant-shaped bottle, repeat the above extraction steps with 20ml of n-hexane-saturated acetonitrile for the remaining n-hexane layer, combine the acetonitrile layer into an eggplant-shaped bottle, and obtain the extract .

[0058] 2) Concentration under reduced pressure: Concentrate the extract obtained in step 1) under reduced pressure in a water bath at 40°C to ab...

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Abstract

The invention discloses a liquid chromatographic detection method of polycyclic aromatic hydrocarbons in edible oil. The liquid chromatographic detection method comprises the following main steps: 1),extracting: weighing a proper amount of sample, putting into a clean centrifuge tube, dissolving the edible oil by using n-hexane saturated by acetonitrile, extracting the polycyclic aromatic hydrocarbons twice by using acetonitrile saturated by n-hexane, and transferring an acetonitrile layer to an eggplant-shaped bottle; 2), concentrating under reduced pressure: concentrating an extract under reduced pressure in a 40 DEG C water bath environment until the volume is about 2ml; 3), performing SPE purification: purifying an obtained concentrate by using an SPE column, and collecting an effluent in a graduated glass tube; 4), performing nitrogen blowing concentration: performing nitrogen blowing concentration on collected liquid at 40 DEG C until the volume is lower than 1ml; 5), fixing thevolume: fixing the volume by using acetonitrile until the volume is 1ml, filtering by using a syringe filter membrane with the thickness of 0.2 microns, and waiting for detection in a sample feedingbottle; 6), detecting and analyzing: analyzing and detecting an obtained solution to be detected by HPLC. By the liquid chromatographic detection method, the operation is simple and quick, the stability is good, the popularizing rate of detection equipment is high, and application is convenient.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and in particular relates to a liquid chromatography detection method for polycyclic aromatic hydrocarbons in edible oil. Background technique [0002] Polycyclic aromatic hydrocarbons (Polycyclic Aromatic Hydrocarbons PAHs) refer to compounds in which two or more benzene rings are connected in the form of fused rings, and are important environmental and food pollutants. Among the more than 200 kinds of polycyclic aromatic hydrocarbons that have been found so far, most of them are heavy polycyclic aromatic hydrocarbons with four to six rings. The International Cancer Research Center (IARC) (1976) lists 94 compounds that are carcinogenic to experimental animals. Among them, 15 kinds belong to polycyclic aromatic hydrocarbons. Since benzo[a]pyrene is the first environmental chemical carcinogen discovered, and its carcinogenicity is very strong, benzo[a]pyrene is often used as the rep...

Claims

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Application Information

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IPC IPC(8): G01N30/06
Inventor 高洪良陈军王锐林俊伶时红张攀仇东朝徐伟
Owner 山东龙大粮油有限公司
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