Dispersed solid-phase extraction material, preparation method and application thereof

Abstract

The invention discloses a dispersed solid-phase extraction material, a preparation method and application thereof, and belongs to the technical field of the detection of aflatoxin in edible oil. The preparation method of the dispersed solid-phase extraction material includes the following steps that: humic acid is weighed and is subjected to ultrasonic washing for 12 to 18 min, and the washed humic acid is subjected to centrifuging, and a solid precipitate is obtained and is dispersed in acetone, and the acetone is subjected to heating and evaporation until the acetone is completely evaporated, and residues are obtained; the residues are taken and arranged in a Soxhlet extractor, and 180 ml of cleaning fluid is added to the Soxhlet extractor, and heating, refluxing and cleaning are performed until a reflux liquid is clear and colorless, and heating is stopped; a cleaned material is taken out, and the material is dried at 100 DEG C for 1.5 to 2.5h, and is cooled for 0.5 to 1h, and thematerial is sieved by a 120-mesh screen, screen underflow is obtained, and the dispersed solid-phase extraction material is obtained. The preparation method disclosed by the invention is suitable formost existing humic acids on the market at present. The preparation method is simple in process and beneficial to control; and the prepared dispersed solid-phase extraction material is stable in property.

Description

technical field

[0001] The invention belongs to the technical field of aflatoxin detection in edible oil, and in particular relates to a dispersed solid-phase extraction material and a preparation method and application thereof. Background technique

[0002] my country is not only a major producer of edible oil but also the largest consumer of edible oil in the world. The annual per capita consumption of edible oil in my country is increasing year by year with the continuous improvement of living standards. Therefore, "edible oil safety" is an important part of "food safety", not only related to the health of the national physique, but also directly affects the development of the national economy.

[0003] Aflatoxins (AFs) are a major pollutant of edible oil, which are secondary metabolites of Aspergillus flavus and Aspergillus parasiticus. So far, a total of 18 AFs have been reported, of which AFB 1 、AFB 2 、AFG 1 and AFG 2 are the four most common. AFs have the charac...

Examples

Embodiment 1

[0037] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0038]S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 15min. Set aside for 8 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 15 minutes, let stand for 8 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the e...

Embodiment 2

[0043] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0044] S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 12min. Set aside for 8 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 12 minutes, let stand for 8 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the ...

Embodiment 3

[0049] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0050] S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 16min. Leave for 7 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 16 minutes, let stand for 7 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the evap...

technical field

[0001] The invention belongs to the technical field of aflatoxin detection in edible oil, and in particular relates to a dispersed solid-phase extraction material and a preparation method and application thereof. Background technique

[0002] my country is not only a major producer of edible oil but also the largest consumer of edible oil in the world. The annual per capita consumption of edible oil in my country is increasing year by year with the continuous improvement of living standards. Therefore, "edible oil safety" is an important part of "food safety", not only related to the health of the national physique, but also directly affects the development of the national economy.

[0003] Aflatoxins (AFs) are a major pollutant of edible oil, which are secondary metabolites of Aspergillus flavus and Aspergillus parasiticus. So far, a total of 18 AFs have been reported, of which AFB 1 、AFB 2 、AFG 1 and AFG 2 are the four most common. AFs have the charac...

Examples

Embodiment 1

[0037] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0038]S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 15min. Set aside for 8 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 15 minutes, let stand for 8 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the e...

Embodiment 2

[0043] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0044] S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 12min. Set aside for 8 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 12 minutes, let stand for 8 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the ...

Embodiment 3

[0049] The application provides a method for preparing a dispersed solid phase extraction material, comprising the following steps:

[0050] S1. Weigh 5g of the humic acid sample sold in China and put it into a 1L beaker, add 500mL of water, fully stir and disperse, put the beaker into an ultrasonic instrument, and perform ultrasonic cleaning. The time of ultrasonic cleaning is 16min. Leave for 7 hours, remove the supernatant, add 500mL of water again, perform ultrasonic cleaning for 16 minutes, let stand for 7 hours, remove the supernatant, repeat the above steps 10 times, until the supernatant has no obvious light yellow phenomenon under natural light; If the particles in the beaker are not completely settled after standing for 8 hours during the standing process of the sample, repeat the above steps for 10 times of cleaning; Min speed, centrifuge for 6min, centrifuge to obtain solid precipitate, transfer the precipitate to a 75mL evaporating dish with acetone, heat the evap...

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