Solid phase extraction column used for measuring saturated hydrocarbon mineral oil in food and preparation method and application of solid phase extraction column

A solid-phase extraction column and mineral oil technology, applied in the field of analytical chemistry and detection, can solve problems such as poor purification effect, large consumption of reagents, cumbersome operation, etc., to save sample processing time, simplify sample processing steps, and save costs Effect

Active Publication Date: 2017-12-12
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Researchers at home and abroad have combined activated alumina, activated silica gel, sulfuric acid silica gel, silver nitrate silica gel and other fillers for the detection of MOSH components in different foods, but there are problems such as cumbersome operation, large consumption of reagents, and poor purification effect.

Method used

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  • Solid phase extraction column used for measuring saturated hydrocarbon mineral oil in food and preparation method and application of solid phase extraction column
  • Solid phase extraction column used for measuring saturated hydrocarbon mineral oil in food and preparation method and application of solid phase extraction column
  • Solid phase extraction column used for measuring saturated hydrocarbon mineral oil in food and preparation method and application of solid phase extraction column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of Composite Porous Filler

[0033] (1) 1% silver nitrate silica gel (operation in dark): Dissolve 0.5g silver nitrate into a round bottom flask filled with 50mL ultrapure water (wrapped with aluminum foil in advance), then add 49.5g silica gel (baked at 600°C 4h), dry and mix in a 70°C water bath under a vacuum of 120mbar for 3h, then put it in a gas chromatograph oven at 125°C for 15h, then put it in a dry container for later use.

[0034] (2) ZSM-5 molecular sieve: drop the NaOH solution into the aluminum sulfate solution, stir evenly as the aluminum source, use silica sol as the silicon source, slowly drop the silicon source into the aluminum source and stir well, then add a certain amount of n-butyl amine. The material ratio of the resulting mixture is n(Na2O): n(SiO2): n(Al2O3): n(H2O)=7: 80: 9.6: 2480. The mixture was aged at room temperature for 12 hours, crystallized at 180°C for 36 hours, cooled naturally, centrifuged, washed with deion...

Embodiment 2

[0036] Example 2 Preparation of Saturated Hydrocarbon Mineral Oil Solid-Phase Extraction Column (Operation in the Dark)

[0037] refer to figure 1 , the solid phase extraction column (1) is made of an open glass column, the inner diameter of the column is 15mm, the column length is 105mm, and a layer of glass fiber filter paper (4) is respectively arranged at the upper, middle and lower positions of the column cavity to separate Form two packing chambers, put glass fiber filter paper (4) in the bottom end of the column, then put 3g self-made 1% silver nitrate silica gel packing (3), after compacting, put glass fiber filter paper (4), and then put 1.75g ​​molecular sieve diatomaceous earth mixed filler (2), and then compacted, that is, the solid phase extraction column is filled.

Embodiment 3

[0038] Example 3 Detection of saturated hydrocarbon mineral oil in edible vegetable oil (operation in dark)

[0039] Weigh 0.50g of different edible vegetable oils (corn germ oil, soybean oil) into two graduated glass test tubes, use isooctane to make the volume to 1.5mL, and pipette 750uL of the sample solution to the Example 2 On the solid-phase extraction column, let the sample slowly infiltrate into the solid-phase extraction column, and let it stand for about 30 minutes, so that the oil sample is completely absorbed by the stationary phase. Rinse the solid-phase extraction column with 2 mL of mixed solution of isooctane and n-heptane (volume ratio: 9:1), and discard the dead volume. Then eluted with 15mL isooctane-n-heptane mixed solution at a flow rate of 1mL / min and collected in a KD concentrator tube to obtain saturated hydrocarbon mineral oil components. Concentrate the saturated hydrocarbon solution to 0.5mL at 30-40°C with nitrogen purging for PTV-GC-FID analysis, an...

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Abstract

The invention relates to a solid phase extraction column used for measuring saturated hydrocarbon mineral oil in a food and a preparation method and application of the solid phase extraction column. The solid phase extraction column comprises a column pipe (1) and composite porous fillers (2, 3) in the column pipe, the column pipe is internally provided with three layers of glass fiber filter paper (4), a cavity of the column pipe is separated into an upper layer filler cavity space and a lower layer filler cavity space, a molecular sieve-diatomite mixed filler is filled in one filler cavity, and a silica gel filler dipped with silver nitrate is filled in another filler cavity. The combination of the solid phase extraction column and gas chromatography-large volume injection is adopted, and a method for detecting the content of the saturated hydrocarbon mineral oil in the food is established. The solid phase extraction column has the advantages of simple and convenient operation, easiness in preparation, low cost, good purifying effect and the like, and is suitable for monitoring the contamination of the saturated hydrocarbon mineral oil in the food in the inspection agencies, the research and development institutions and the food enterprises.

Description

technical field [0001] The invention relates to the technical fields of analytical chemistry and detection, and more particularly relates to a solid-phase extraction column for the determination of saturated hydrocarbon mineral oil and its application in the detection of saturated hydrocarbon mineral oil content in food. Background technique [0002] Mineral oil hydrocarbon (MOH) is a kind of extremely complex hydrocarbon mixture, its carbon number is generally between 10-50, mainly including saturated hydrocarbon mineral oil (MOSH) composed of linear, branched and cyclic alkanes ) and mineral oil of aromatic hydrocarbons (MOAH) composed of alkylated polyaromatic compounds. Hydrocarbon mineral oil is the pollutant with the largest accumulation in the human body. Hydrocarbon mineral oil containing toxic components will migrate into food, accumulate in organisms at all levels after dietary intake, and eventually threaten human health through the food chain. Due to the potenti...

Claims

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Application Information

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IPC IPC(8): B01D15/20B01D15/22G01N30/02G01N30/06
CPCB01D15/206B01D15/22G01N30/02G01N30/06G01N2030/062
Inventor 柯润辉杨春艳尹建军宋全厚安红梅王丽娟
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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