Benzo(a)pyrene from Smoked Meat Products Aromatised with Artificial Smoke Aroma

Benzo[a]pyrene from Smoked Meat Products Aromatised with Artificial Smoke Aroma

Method:	Matrix	Application-No.:
SPE	meat	302720

Substances:

benzo[a]pyrene

Column:

CHROMABOND^® CN/SiOH, 6 ml, 500/1000 mg

Phase:

CHROMABOND^® CN/SiOH

REF number:

730135

Sample pretreatment:

The meat sample (at least 100 g) is homogenised with a suitable device. 20 g of the homogenised sample are weighted on a folded filter and inserted into an extraction thimble. Add 1 mL benzo[b]chrysene standard solution and put the extraction thimble in a Soxhlet extractor. Fill the Soxhlet flask with 200 mL methanol and 25 mL potassium hydroxyde solution (50 %). Extract the sample for 5 hours on a sand or water bath. The extraction fluid must boil.

Add 150 mL n-hexane to the cold extract and stirr with a magnetic stirrer for 1 hour. Then add 100 mL dest. water and give all of the extract into an extraction funnel. Rinse the Soxhlet two times with 10 mL methanol.

After phase separation collect the hexane phases and wash the aqueous phase two times with 100 mL n-hexane. The combined n-hexane phases are dried over sodium sulphate.

Conditions:

Conditioning: 5 mL dichloromethane and then 5 mL cyclohexane

Sample application: The hexane phase is dried with a rotation evaporator at 40 °C. The residue is dissolved in 1 mL cyclohexane an applied on the activated column.

Washing: 2 x 2 mL n-hexane, suck air through the column until it is dry

Elution: 5 x 5 mL acetonitrile

Concentration: Evaporate to dryness with a rotation evaporator at 40 °C. The residue is dissolved in 1 mL acetonitrile. The solution is filtered through a membrane filter (0.45 μm, e.g. CHROMAFIL^® PET, REF 729023) or centrifugated with an ultra centrifuge.

Subsequent analysis:

HPLC with NUCLEOSIL^® 100-5 C18 PAH
(Please see also modern NUCLEODUR^® C18 PAH)

Author(-s):

Hartmann, K.

Source:

Landesuntersuchungsamt Rheinland-Pfalz, Fachbereich Tiermedizin, Koblenz, Germany

Keywords:

benzopyrene; PAHs; smoked meat

Recovery rates:

	recovery rate (μg/kg)	recovery rate (%)
primary contamination: 0.013 μg/kg
addition (1): 0.013 + 0.025 μg/kg	0.033	87
addition (2): 0.013 + 0.050 μg/kg	0.049	78

Comment:

Recovery rates were determined by addition of two benzo(a)pyrene concentrations to the sample material.

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