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Separation column filler for separating PCBs (Poly Chlorinated Biphenyls) or OCPs (Organic Chlorine Pesticides) in high-fat content sample and separation method

A separation column and separation instrument technology, which is applied in the packing field of chromatography separation column, can solve the problems of unsatisfactory purification effect, long separation time, cumbersome separation method, etc., achieve good separation effect, improve separation effect, and simple separation method Effect

Inactive Publication Date: 2013-10-02
DALIAN MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the separation of PCBs or OCPs in animal tissue samples, although column chromatography has a good recovery rate and purification effect, the purification effect of some of them is not ideal, such as organochlorine pesticides (OCPs) containing certain extremes. The recovery rate of methoxychlor and δ-HCH will become worse. The conventional way to improve it is to increase the amount of eluent, or increase the polarity of eluent appropriately, resulting in a large amount of solvent and long separation time. and other shortcomings [3]
For samples with high fat content, because of the complex matrix, the separation of PCBs or OCP in the sample requires special treatment, the separation method is cumbersome, the separation time is long, and the recovery rate is low

Method used

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  • Separation column filler for separating PCBs (Poly Chlorinated Biphenyls) or OCPs (Organic Chlorine Pesticides) in high-fat content sample and separation method
  • Separation column filler for separating PCBs (Poly Chlorinated Biphenyls) or OCPs (Organic Chlorine Pesticides) in high-fat content sample and separation method
  • Separation column filler for separating PCBs (Poly Chlorinated Biphenyls) or OCPs (Organic Chlorine Pesticides) in high-fat content sample and separation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Separation of PCBs mixture by Seitz four-channel chromatographic separator

[0041] The separation column packing pretreated according to the above method was filled in the special separation column of the Seitz four-channel chromatographic separation instrument (Seitz Technology (Dalian) Co., Ltd.), and the mixed solution of n-hexane and dichloromethane was used as the mobile phase. Separate the sample solution containing 21 kinds of PCBs, the specific method is as follows:

[0042] (1) Preparation of separation column packing

[0043] Weigh the silica gel pretreated by the above method, concentrated sulfuric acid modified silica gel, florisil and anhydrous sodium sulfate, wherein the particle size of silica gel is 200-300 mesh, and the particle diameter of acid modified silica gel is 100-200 mesh , Florisil particle size 60-100 mesh. Mix silica gel and florisil at a mass ratio of 1:1 and stir evenly to obtain a silica gel-florisil mixture.

[0044] (2) Co...

Embodiment 2

[0064] Example 2 Separation of PCBs mixture in fish tissue by Seitz four-channel chromatographic separator

[0065] (1) Sample extraction

[0066] Fish tissue samples were weighed (the samples were freeze-dried before the experiment) and divided into experimental group 1 and experimental group 2. Experimental group 1 was set up with 8 parallel tests, and experimental group 2 was set with 4 parallel tests. Add 5g of fish tissue to the Erlenmeyer flask for each experimental group, and add 1ml of PCBs mixed standard solution with a concentration of 50ppb to the Erlenmeyer flask of experimental group 1. Add acetone / petroleum ether (V 1 / V 2 =1 / 1) 20ml, collect the extract after ultrasonic extraction at 25°C for 15min, filter the extract through a funnel filled with anhydrous sodium sulfate, and collect it in an Erlenmeyer flask. Then use a small amount of acetone / petroleum ether ((V 1 / V 2 =1 / 1) solution rinses the anhydrous sodium sulfate in the funnel, repeats the above ext...

Embodiment 3

[0086] Example 3 Seitz Four-channel Chromatographic Separator Separation of OCPs Mixture

[0087] (1) Preparation and packing of separation column

[0088] Operate according to the method of (1)-(2) in Example 1.

[0089] (2) Equilibrium separation column

[0090] Add 2ml of n-hexane-dichloromethane (20:80) to the upper end of the separation column once, and elute at an elution pressure of 75kpa. The elution time is 50s, and the elution is repeated 7-9 times to make the separation column reach equilibrium.

[0091] (3) Separation

[0092] After the separation column is balanced, slowly add 1ml of OCPs mixed standard solution (containing 22 kinds of OCPs components as shown in Table 3, organic chlorine (OCPs) mixed standard of Accstandard Company of the United States) with a concentration of 50ppb to the upper end of the separation column, and use n-hexane-dichloro The mixed solution with methane ratio of 20:80 was eluted, the elution pressure was 75kpa, the elution time was...

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Abstract

The invention discloses a separation column filler for separating PCBs (Poly Chlorinated Biphenyls) or OCPs (Organic Chlorine Pesticides) in a high-fat content sample and a separation method. The filler is composed of 30%-35% of silica gel-florisil mixture, 50%-60% of acidic modified silica gel and 10%-15% of anhydrous sodium sulfate, by weight percentage. The separation column filler provided by the invention can be filled in a separation column for conventional column chromatography or a Seitz four-channel chromatographic separator, and used for chromatographic separation with the mixed solution of normal hexane and dichloromethane as a mobile phase. With the filler provided by the invention to separate the PCBs or the OCPs, the separation method is efficient, quick and simple in process; an obvious separation effect can be achieved under the condition of low cost; the column recovery rate of the PCBs materials is in the range from 93% to 105% and adding standard recovery to fish tissues is in the range from 74% to 100%; and the column recovery rate of the OCPs materials is in the range from 77% to 120% and adding standard recovery to fish tissues is in the range from 78% to 102%.

Description

technical field [0001] The invention relates to a chromatographic separation column packing, in particular to a separation column packing for separating PCBs or OCPs in samples with high fat content and a method for using the packing to separate PCBs or OCPs in fat-containing animal tissue samples. Background technique [0002] Under current technical conditions, there are three commonly used methods for purification in the pretreatment process of high-fat samples: solid phase extraction (SPE), gel permeation chromatography (GPC) and chromatography. [0003] The solid phase extraction (SPE) process can be divided into two parts: adsorption and elution. During the adsorption process, the target substance is selectively adsorbed on the adsorption bed for enrichment. During this process, due to the existence of co-adsorption, adsorbent selectivity and other factors, some substances that interfere with the determination of PCBs and OCPs will also be adsorbed on the adsorption b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/20B01D15/10G01N30/14
Inventor 李清波蒋培宇
Owner DALIAN MARITIME UNIVERSITY
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