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A sample pretreatment method for detecting organochlorine in milk and a detection method using it

An organochlorine and milk technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to meet the detection requirements, low recovery rate of organochlorine components, long gel chromatography column packing and column passing time, etc. , to achieve the effect of simple and fast recovery rate and improve efficiency

Active Publication Date: 2016-04-06
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"GB / T5009.162-2008 Determination of Multi-Component Residues of Organochlorine Pesticides and Pyrethroid Pesticides in Animal Food" and "GB / T5009.19-2008 Determination of Multi-Component Residues of Organochlorine Pesticides in Food" The milk pretreatment method provided in the article is as follows: first extract with acetone and petroleum ether, concentrate and then purify by gel chromatography, because the time for packing and passing through the column of gel chromatography in this pretreatment method is too long, it cannot meet the requirements. Purpose of instant and rapid detection
The milk pretreatment method provided in "GB / T23210-2008 Determination of 511 Pesticides and Related Chemical Residues in Milk and Milk Powder by Gas Chromatography-Mass Spectrometry" is: acetonitrile extraction, rotary evaporation concentration, and ENVI-18 solid phase Purify the extraction column, wash the sample bottle with acetonitrile, put the washing liquid in the solid phase extraction column, and exchange the eluent with n-hexane for solvent exchange. The recovery rate of some organic chlorine components is low in the previous treatment method, such as trans - Chlordane, heptachlor, p,p'-DDD, α-endosulfan, etc., cannot meet the testing requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

no. 1 example

[0018] The first embodiment: a pre-processing method.

[0019] 1. Instruments, consumables and reagents:

[0020] Rotary evaporator: equipped with vacuum system and heating device;

[0021] Nitrogen blower and centrifuge;

[0022] n-hexane-acetone mixture (9:1): mixed n-hexane and acetone at a volume ratio of 9:1;

[0023] Sodium chloride and magnesium sulfate are analytically pure; organic solvents are chromatographically pure, and the experimental water meets the requirements of GB / T6682 tertiary water;

[0024] Flori diatomite solid phase extraction column: 500mg / 3mL, the activation method is to rinse the Flori diatomite solid phase extraction column with 3mL n-hexane and 3mL n-hexane-acetone mixture (9:1) in sequence.

[0025] 2. Method steps:

[0026] a. Take 10 grams of milk in a 50mL centrifuge tube, add 20ml of acetonitrile, 4g of magnesium sulfate and 1g of sodium chloride, vortex and mix for 1 minute, and centrifuge at 4000 rpm for 5 minutes; then use a dropper ...

no. 2 example

[0031] The second embodiment: a pre-processing method.

[0032] 1. Instruments, consumables and reagents:

[0033] The instruments, consumables and reagents are the same as those described in the first embodiment.

[0034] 2. Method steps:

[0035] a. Take 10 grams of milk in a 50mL centrifuge tube, add 25ml of acetonitrile, 3g of magnesium sulfate and 1.5g of sodium chloride, vortex and mix for 1.5 minutes, centrifuge at 5000 rpm for 4 minutes; then use a dropper Transfer all the organic phase (i.e. the supernatant after centrifugation) to a 250mL rotary evaporating flask, and rotary evaporate to dryness in a water bath at 55°C;

[0036] b. Clean the rotary evaporator flask with 2 ml of acetonitrile, 4 ml of water and 2 ml of acetonitrile in turn, and transfer to a 50 ml centrifuge tube to combine to obtain the cleaning solution;

[0037] c. Add n-hexane equal to the volume of the cleaning solution to the cleaning solution, vortex and mix for 45 seconds, transfer the org...

no. 3 example

[0040] The third embodiment: a pre-processing method.

[0041] 1. Instruments, consumables and reagents:

[0042] The instruments, consumables and reagents are the same as those described in the first embodiment.

[0043] 2. Method steps:

[0044] a. Take 10 grams of milk in a 50mL centrifuge tube, add 30ml of acetonitrile, 5g of magnesium sulfate and 2g of sodium chloride, vortex and mix for 2 minutes, and centrifuge at 6000 rpm for 8 minutes; then use a dropper Transfer all the organic phase (i.e. the supernatant liquid after centrifugation) to a 250mL rotary evaporating flask, and rotary evaporate to dryness in a water bath at 60°C;

[0045] b. Clean the rotary evaporating flask with 3 ml of acetonitrile, 6 ml of water and 3 ml of acetonitrile in turn, and transfer to a 50 ml centrifuge tube to combine to obtain the cleaning solution;

[0046] c. Add n-hexane equal to the volume of the cleaning solution to the cleaning solution, vortex and mix for 60 seconds, transfer ...

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PUM

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Abstract

The invention provides a sample pretreatment method for detecting organochlorine in milk, comprising: a. extracting the milk with acetonitrile, taking the organic phase and rotating it to dryness; b. cleaning the container of the rotating evaporation with acetonitrile, water and acetonitrile in sequence , to obtain the cleaning solution after merging; c, carry out normal hexane extraction to the cleaning solution, take the organic phase and dry it with nitrogen; d, dissolve the substance obtained by drying the nitrogen in step c, and then purify it with a solid phase extraction column; e, purify The resulting liquid nitrogen was blown to dryness, and then dissolved with n-hexane. Wherein, the container of rotary evaporation is cleaned with acetonitrile, water and acetonitrile in sequence, and the components to be tested adsorbed on the container wall can be recovered more fully. The sample pretreatment method is simple, fast and has a high recovery rate. The present invention also provides a method for detecting organochlorine in milk by pre-treating the milk through the sample pre-treatment method.

Description

technical field [0001] The invention relates to a sample pretreatment method for detecting organic chlorine and a detection method using the method, and is especially suitable for detecting organic chlorine in milk. Background technique [0002] There is a risk of organochlorine contamination during milk production. Common organochlorines include α-666, β-666, γ-666, δ-666, p,p'-DDE, p,p'-DDD, o, p'-DDT, p,p'-DDT, heptachlor, epoxyheptachlor, cis-chlordane, trans-chlordane, oxychlordane, β-endosulfan, endosulfan sulfate, dieldrin , Aldrin, etc. [0003] Several methods for the detection of organochlorines in milk have been developed. "GB / T5009.162-2008 Determination of Multi-Component Residues of Organochlorine Pesticides and Pyrethroid Pesticides in Animal Food" and "GB / T5009.19-2008 Determination of Multi-Component Residues of Organochlorine Pesticides in Food" The milk pretreatment method provided in the article is as follows: first extract with acetone and petroleum e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08
Inventor 姜瑞清常建军魏文平曹海霞周琳宋晓东
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD