Sample Testing Process

Sample Pretreatment Process

Step 1 Homogenization

● Weigh 25g fruit or vegetables sample in each 100ml centrifuge tube;

● Add 50ml acetonitrile;

● Preset parameters 5000r/min; 2min;

● With filter paper, collect 50ml sample into a graduated cylinder containing 5-7g of sodium chloride;

● Put on test tube caps and take balanced vibration;

● Let stand for a while until the acetonitrile is separated from water.

Step 2 Sample Pre-concentration

● Take 10ml supernatant into a test tube or beaker;

● Adjust the water temperature to 60℃and start nitrogen blowing;

● Add 2.0ml organic solvent and cover with aluminum foil;

● Organic solvents for reference:

Organophosphorus—2.0ml acetone

Organochlorine and pyrethroid—2.0ml n-hexane

Carbamate—2.0ml methanol : dichloromethane (1:99)

Step 3 Extraction & Purification

Organophosphorus

(No need for this step)

Organochlorine and Pyrethroid

(Flory silica column: 6ml; 1000mg)

Pretreatment

5ml acetone : n-hexane (10:90), 5ml n-hexane rinse the activated extraction column sequentially and discard the effluent.

Sample Passing Column

When liquid level of the activated eluent drops to the surface of the filler, ensure that the filler is wet and immediately pour 2ml sample to be purified. At the same time rinse sample tube with 5ml acetone : n-hexane (10:90) , then repeat once and pour it into inlet column for purification.

Eluent Receiving

Use a 15ml centrifuge tube to receive the eluate through the column, then wait for nitrogen blowing to 5ml.

Carbamate

(Amino column: 6ml; 500mg)

Pretreatment

4ml methanol : dichloromethane (1:99) rinse the extraction column and discard the effluent.

Sample Passing Column

When pretreatment solvent reaches the surface of filler adsorption layer, immediately pour 2ml sample to be purified. At the same time, rinse sample tube with 2ml methanol : dichloromethane (1:99), then repeat once and pour it into inlet column for purification.

Eluent Receiving

Use a 15ml centrifuge tube to receive the eluate through the column, then wait for nitrogen blowing to 5ml.

Step 4 Concentration & Settling

Organophosphorus

Transfer concentrated 2ml sample to a 15ml centrifuge tube;

Elute the sample tube with 3ml acetone several times, then transfer it to a 15ml centrifuge tube;

Add acetone to 5ml, vibrate and mix, then transfer sample to two 2ml vials.

Organochlorine and Pyrethroid

Sample is blown by nitrogen to below 5ml with water temperature 50℃.

Add n-hexane to 5ml, vibrate and mix, then transfer sample to two 2ml vials.

Carbamate

Sample is blown by nitrogen to nearly-dry status with water temperature 50℃.

Add methyl alcohol to 2.5ml, vibrate and mix, then filter sample with 0.2μm filter membrane.

Next, it’s turn to analyze sample by GC/LC technology......

REF:

https://www.scienceofcooking.com/maillard_reaction.htm

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