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Method for detecting benzopyrene (a) in lubricating oil (grease)

A detection method and lubricating oil technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex matrix, inability to achieve effective detection, matrix interference, etc., to reduce interference, easy to detect large quantities of samples, and high accuracy Effect

Active Publication Date: 2012-07-04
CHENGUANG BIOTECH GRP CO LTD
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  • Claims
  • Application Information

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Problems solved by technology

Because the matrix of lubricating oil (grease) is complex, it contains not only base oil but also thickener and additives, so the above-mentioned detection method of BaP in food is directly used, the matrix interference is very large, and effective detection cannot be realized

Method used

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  • Method for detecting benzopyrene (a) in lubricating oil (grease)
  • Method for detecting benzopyrene (a) in lubricating oil (grease)
  • Method for detecting benzopyrene (a) in lubricating oil (grease)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: The specific steps of the detection method of benzo(a)pyrene in this lubricating oil (grease) are as follows.

[0030] (1) Standard curve: Accurately weigh 10 mg (accurate to 0.1 mg) of BaP standard substance in a 100 mL volumetric flask, dissolve with methanol and constant volume, and make 0.1 mg·mL -1 standard stock solution. Its working curve is gradually diluted from the standard stock solution to a mass concentration of 5.0, 10.0, 50.0, 100.0, 150.0, 200.0 μg L -1 A series of standard solutions were injected according to the above test conditions to make a standard curve for analysis.

[0031] (2) Sample extraction: Accurately weigh 1.0g (accurate to 0.0001g) of grease sample into a 25mL volumetric flask, add 10mL of cyclohexane-ethyl acetate (1:1, v / v) mixed solution, ultrasonic for 15min, Cool to room temperature, add cyclohexane-ethyl acetate (1:1, v / v) mixed solution to make up to volume. The extract was transferred to a centrifuge tube, centri...

Embodiment 2

[0040] Embodiment 2: The specific steps of the detection method of benzo(a)pyrene in this lubricating oil (grease) are as follows.

[0041] (1) Standard curve: Accurately weigh 10 mg (accurate to 0.1 mg) of BaP standard substance in a 100 mL volumetric flask, dissolve in methanol and constant volume, and make 0.1 mg·mL -1 standard stock solution. Its working curve is gradually diluted from the standard stock solution to a mass concentration of 5.0, 10.0, 50.0, 100.0, 150.0, 200.0 μg L -1 A series of standard solutions were injected according to the above test conditions to make a standard curve for analysis.

[0042] (2) Sample extraction: Accurately weigh 1.5 g (accurate to 0.0001 g) of lubricating oil sample into a 20 mL volumetric flask, add 10 mL of cyclohexane-ethyl acetate (1:1, v / v) mixed solution, and ultrasonically After 10 min, cool to room temperature, add cyclohexane-ethyl acetate (1:1, v / v) mixed solution to make up to volume. The extract was transferred to a c...

Embodiment 3

[0047] Embodiment 3: The specific steps of the detection method of benzo(a)pyrene in this lubricating oil (grease) are as follows.

[0048] (1) Standard curve: Accurately weigh 10 mg (accurate to 0.1 mg) of BaP standard substance in a 100 mL volumetric flask, dissolve with acetonitrile and make up to 0.1 mg·mL -1 standard stock solution. Its working curve is gradually diluted from the standard stock solution to a mass concentration of 5.0, 10.0, 50.0, 100.0, 150.0, 200.0 μg L -1 A series of standard solutions were injected according to the above test conditions to make a standard curve for analysis.

[0049] (2) Sample extraction: Accurately weigh 0.5 g (accurate to 0.0001 g) of grease sample into a 10 mL volumetric flask, add 5 mL of cyclohexane-ethyl acetate (1:1, v / v) mixed solution, and ultrasonically 3 times, 30 min each time, cooled to room temperature, and distilled cyclohexane-ethyl acetate (1:1, v / v) mixed solution to volume. The extract was transferred to a centri...

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Abstract

The invention discloses a method for detecting benzopyrene (a) in lubricating oil (grease). The method comprises the following steps: after extracting and centrifuging lubricating oil (grease) and purifying the lubricating oil (grease) through gel permeation chromatography, collecting a target eluent and concentrating till the target eluent is dry; stabilizing volume, thereby obtaining a sample solution; and lastly, detecting the sample solution according to a reversed-phase high performance liquid chromatography-fluorescence method and quantifying according to an external standard method. According to the method, a GPC (Gel Permeation Chromatograph) purifying technology is adopted for processing the lubricating oil (grease), majority macromolecular oily impurities are removed, the interference of a sample substrate to BaP (Benzo A Pyrene) measurement is greatly reduced, and the detecting method is high in accuracy and strong in applicability to the lubricating oil (grease). The GPC purifying technology and the reversed-phase high performance liquid chromatography-fluorescence method are used together for detecting, so that the whole process is high in automaticity and is convenient and quick and the detection for mass samples is easily realized. The waste liquid generated during the GPC purifying process is recyclable and reusable; the detection cost is lowered; and the environmental pollution is reduced.

Description

technical field [0001] The invention relates to a detection technology for toxic substances in lubricating oil (fat) during food processing, in particular to a detection method for benzo(a)pyrene in lubricating oil (fat). Background technique [0002] Benzo[a]pyrene (BaP) is one of the most representative polycyclic aromatic hydrocarbon compounds, and is considered to be one of the world's three strong carcinogens, and it is the key monitoring and control of national food safety work object. It is generally believed that BaP in food mainly comes from the cooking process of food itself, pollution in processing and packaging links, and food environmental pollution. Among them, there are many research reports on the production mechanism of BaP in the process of food smoking and baking, and the BaP air pollution caused by the combustion of coal, gasoline, tobacco and other substances, and the pollution of food contact materials in the process of processing, and due to Food BaP...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 连运河高伟吉桂珍王磊程淑君
Owner CHENGUANG BIOTECH GRP CO LTD
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