GB/T 23504-2009Determination of zearalenone in food -- High performance liquid chromatographic method with immunoaffinity column clean-up (English PDF)

5.5 Glass syringe. 10 mL.

5.6 Test screen. 1 mm aperture.

5.7 Air pressure pump.

6.1 Sample preparation and extraction

6.1.1 Food and grain products. GRIND samples; USE high-speed universal mill

to grind the hard grain and MAKE it pass the test sieve (5.6); DO not grind it

into powder. WEIGH 50 g of ground test specimen (accurate to 0.01 g) and

PLACE it into a 100 mL volumetric flask; ADD 5 g of sodium chloride; USE the

extraction solution (4.3) to make its volume reach to the mark; MIX it uniformly;

TRANSFER it into a homogeneous cup; MAKE it subjected to high-speed

stirring and extraction for 2 min. USE the quantitative filter paper to filter it;

TRANSFER 10.0 mL of filtrate into a 50 mL volumetric flask; ADD water to make

its volume reach to the mark; MIX it uniformly; USE glass fiber filter paper to

the filter it until the filtrate is clean; COLLECT the filtrate A into a clean container.

6.1.2 Alcohols. TAKE 20 g of alcohol samples (the alcohol containing carbon

dioxide is refrigerated at 4 °C for 30 min, filtered or degassed ultrasonically prior

to use) or other alcohol samples containing no carbon dioxide (accurate to 0.01

g) into a 50 mL volumetric flask; USE acetonitrile to make its volume reach to

the mark; SHAKE it uniformly; TRANSFER 10.0 mL of filtrate into a 50 mL

volumetric flask; ADD water to make the volume reach to the mark; MIX it

uniformly; USE glass fiber filter to filter it until the filtrate is clean; COLLECT the

filtrate B into a clean container.

6.1.3 Soy sauce, vinegar, sauce and sauce products. WEIGH 25 g (accurate to

0.01 g) of uniformly mixed test specimen; USE acetonitrile to make the volume

reach to 100.0 mL; MAKE it subjected to ultrasonic extraction for 2 min; USE

the quantitative filter paper to filter it; TRANSFER 10.0 mL of filtrate into a 50

mL volumetric flask; ADD water to make the volume reach to the mark; MIX it

uniformly; USE glass fiber filter to filter it until the filtrate is clean; COLLECT the

filtrate C into a clean container.

6.2 Purification

CONNECT the immunoaffinity column to under the glass syringe (5.5);

accurately PIPETTE 10.0 mL of the filtrate A or B or C as mentioned in 6.1 into

the glass syringe. CONNECT the air pressure pump to the glass syringe;

ADJUST the pressure so that the solution can pass through the immunoaffinity

......