GB 5009.27-2016National food safety standard - Determination of Benzo(a)Pyrene in Foods (English PDF)

3.1 Reagents

3.1.1 Toluene (C7H8). Chromatographically pure.

3.1.2 Acetonitrile (CH3CN). Chromatographically pure.

3.1.3 n-hexane (C6H14). chromatography.

3.1.4 Dichloromethane (CH2Cl2). Chromatographically pure.

3.2 Standards

Benzo(a)pyrene standard (C20H12, CAS No.. 50-32-8). the purity shall be >= 99.0%; or solution into the chromatograph’s sample vial again; concentrate it until it is near dry.

Accurately pipette 1mL of acetonitrile into the chromatograph’s sample vial, vortex re- dissolve it for 0.5min; after passing the microporous membrane, it shall be used for liquid chromatography.

Purification method 2. adopt the benzo(a)pyrene molecular imprinting column; orderly use 5mL of dichloromethane and 5mL of n-hexane to activate the column. Transfer the liquid to be purified into the column; when the liquid-level falls to the column bed, use

6mL of n-hexane to rinse the column; discard the effluent. Use 6mL of dichloromethane to elute and collect the purified solution into the test tube. Under 40°C, use nitrogen to dry the purification solution; accurately pipette 1mL of acetonitrile; vortex re-dissolve it for 0.5min; after passing the microporous membrane, it shall be used for liquid chromatography.

5.1.2 Smoked, roasted & barbecued AND smoked & grilled aquatic products

Pretreatment. remove the bones of the meat; remove the thorns of fish; remove the shell of shellfish; grind the edible portion evenly; store it in clean sample bottles; mark it; at -16°C ~ -18°C, stored it in the refrigerator.

Extraction. same as the extraction in 5.1.1.

Purification method 1. Except that the volume of n-hexane’s eluent is 70 mL, the rest of the operation shall be the same as the purification method 1 in 5.1.1.

Purification method 2. the operation shall be the same as the purification method 2 in

5.1.1.

5.1.3 Grease and its products

Extraction. weigh and take 0.4g (accurate to 0.001g) of sample; add 5mL of n-hexane;

vortex-mix it for 0.5min. To be purified.

Note. If the samples are the hydrous oil products, such as margarine, etc., emulsification will occur. It shall perform 4000r/min centrifugalization for 5min; transfer out the n-hexane layer. To be purified.

Purification method 1. Except for using 0.4mL of acetonitrile to vertically re-dissolve the sample in the last, other operations shall be the same as the purification method 1 in 5.1.1.

Purification method 2. Except for using 0.4mL of acetonitrile to vertically re-dissolve the sample in the last, other operations shall be the same as the purification method 2 in 5.1.1. When the sample is prepared, pretreatments of different samples need to have sample’s blank test at the same time.

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