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Two-step separation-purification column and use thereof

A purification column and packing column technology, applied in the chemical field, can solve the problems of low PAEs, large difficulty, complex matrix, etc., and achieve high application value and easy detection

Inactive Publication Date: 2009-09-16
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low content of PAEs in food samples and the complex matrix, it is difficult to accurately analyze and measure them. The current difficulty in analysis and determination is the pretreatment of samples.

Method used

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  • Two-step separation-purification column and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Polyvinyl chloride (PVC) film was cut into 0.5 cm x 0.5 cm pieces. Weigh 0.500g of film, add 1.96mg / kg DNOP standard solution and 2.094mg / kg DBP standard solution. Add 30ml of n-hexane, sonicate for 30min, wash the residue with 20ml of n-hexane for 3 times, combine the washings, concentrate to 3-5ml by rotary evaporation, and carry out subsequent operations.

[0030] ①No column: Blow dry directly with nitrogen blower, dilute to 1ml with methanol, measure the concentration of DNOP and DBP, and calculate the recovery rate;

[0031] ② Activated carbon column: Add about 0.500g of activated carbon particles, first pre-wash the column with 2ml of dichloromethane, then pre-wash the column with 2ml of n-hexane, then load the sample, elute with 5ml of dichloromethane, collect the eluate, Blow dry with a nitrogen blower, dilute to 1ml with methanol, measure the concentration of DNOP and DBP, and calculate the recovery rate;

[0032] ③Through Florisil column: Add 1.500g of Flori...

Embodiment 2

[0039] After the apples were washed and crushed in a high-speed tissue grinder, 15.00 g was weighed, and 0.327 mg / kg of DNOP standard solution and 0.2327 mg / kg of DBP standard solution were added. Add 50 mL of extract solution (V (acetone): V (n-hexane) = 1:3), ultrasonically extract for 1 h, and suction filter to discard the residue. Wash the suction filter flask and funnel with 10 mL of extract, transfer the filtrate to a separatory funnel, collect the organic phase, extract the aqueous phase twice with 50 mL of n-hexane, and combine the organic phases. After concentrating to 3-5ml by rotary evaporation, follow-up operations were performed.

[0040] ①No column: Blow dry directly with nitrogen blower, dilute to 1ml with methanol, measure the concentration of DNOP and DBP, and calculate the recovery rate;

[0041] ② Activated carbon column: Add about 0.500g of activated carbon particles, first pre-wash the column with 2ml of dichloromethane, then pre-wash the column with 2ml ...

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Abstract

The invention provides a two-step separation-purification column and use thereof, relating to separation-purification column and the use of separating and purifying Reomol in food safety testing. The column is made by activated carbon particle filled column at the upper end and Rory silica filled column at the lower end. The two-step separation-purification column is used for separating and purifying Reomol. The invention combines the activated carbon particle column and Rory silica column to purify and enrich di-n-octyl phthalate (DNOP) and di-n-butyl phthalate (DBP), which can reduce the detection limit of the detection limit coarse extract. The detection limit of the DNOP and DBP in the membrane coarse extract is ten times that that purified and enriched by the activated carbon particle column and Rory silica column; the detection limit of the DNOP and DBP in the apple coarse extract is 8.3 times and ten times than that purified and enriched by the activated carbon particle column and Rory silica column. The invention is easy for detecting a large number of samples in large scale.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a food detection method, especially a pretreatment method for food safety detection, specifically a two-step separation and purification column and its application for separating and purifying phthalates in food safety detection. Background technique [0002] Phthalic acid esters (PAEs), also known as phthalates, are commonly used as plasticizers and softeners in the plastics industry, and their content can sometimes be as high as 60% of the polymer itself to increase the plastic's Plasticity and toughness. Both di-n-octyl phthalate (DNOP) and di-n-butyl phthalate (DBP) are phthalates, which are currently widely used plasticizers, with reproductive toxicity, embryotoxicity and genetic Toxicity, they play a role similar to estrogen in humans and animals, interfere with endocrine, and when the content is high, it is considered that they may damage the human liver, kidneys and repr...

Claims

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Application Information

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IPC IPC(8): B01J20/20C07C69/80C07C67/56
Inventor 王向阳姜丽佳施青红
Owner ZHEJIANG GONGSHANG UNIVERSITY
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