Recently, 6 instant noodles produced in Korea by the well-known instant noodle brand Nongshim have been involved in the carcinogen benzopyrene, and the news has aroused great concern from all walks of life. Benzopyrene is a highly active indirect carcinogen produced by carbohydrates, proteins and fats when it is not completely burned. Studies have shown that benzopyrene can cause lung cancer, liver cancer, gastrointestinal cancer, etc., and is a primary carcinogen. Benzopyrene is widely found in foods such as smoked, fried, grilled, and baked goods. The EU and WHO have set benzopyrene for smoked foods not to exceed the upper limit of 5ppb and 10ppb.

In China's "GB 17400-2003 Hygienic Standard for Instant Noodles", there is no standard for the content of p-benzopyrene, but China's "GB 2762-2005 Limits of Contaminants in Foods" clearly stipulates that the edible oil standard does not exceed 10ppb, and the smoked barbecue does not exceed 5ppb , The grain does not exceed 5ppb. This is actually consistent with the standards set by the European Union and WHO. Dima Technology has previously developed a special solid phase extraction column-ProElut BaP for the detection of benzopyrene in vegetable oils and aquatic products, and users have reported good results after use. On this basis, Dima Technology has developed a detection solution for benzopyrene in instant noodles. ProElut BaP has been used to successfully detect benzopyrene in instant noodles. It has the characteristics of good purification effect, stable recovery rate, and simple operation steps.

The following is a detailed solution for your reference!

Detection of benzopyrene in instant noodles

1 Scope of application

It is suitable for the detection of benzopyrene in instant noodles.

2. Instant noodle seasoning package

2.1 Sample extraction

Weigh 0.4 g sample to the nearest 0.001 g, dissolve and dilute with 5 mL of n-hexane, and use it as the sample solution to be purified.

2.2 SPE column purification-ProElut BaP 22 g / 60 mL (Cat. #: 65351)

(1) Activation: 30 mL of n-hexane, the effluent is discarded;

(2) Sample loading: add the liquid to be purified to the small column and collect the effluent;

(3) Rinse: rinse with 50 mL of n-hexane, collect the effluent and combine the effluent from steps (2) and (3)

(4) Redissolve: Distilled under reduced pressure at 30 ℃ * The collected solution was evaporated to dryness, and the volume of acetonitrile-tetrahydrofuran (9: 1) solution was adjusted to 1 mL for HPLC analysis.

3 instant noodle cakes

3.1 Sample extraction

(1) Weigh 1 g sample into a 50 mL centrifuge tube and add 15 mL of n-hexane.

(2) Vortex to mix for 2 min, ultrasonic extraction for 5 min, centrifuge at 6000 rpm for 3 min, and collect supernatant;

(3) Extract the residue with 15 mL of n-hexane, mix for 2 min each time with vortex, extract with ultrasound for 5 min, and centrifuge at 5000 rpm for 3 min; combine the two extracts;

(4) Distilled under reduced pressure at 30 ℃ * The extract is evaporated to dryness, then dissolved with 5 mL of n-hexane, to be purified.

3.2 SPE column purification-ProElut BaP 22 g / 60 mL (Cat. #: 65351)

(1) Activation: 30 mL of n-hexane, the effluent is discarded;

(2) Sample loading: add the liquid to be purified to the small column and collect the effluent;

(3) Rinse: 70 mL of n-hexane rinse, collect the effluent and combine the effluent from steps (2) and (3);

(4) Redissolve: Distilled under reduced pressure at 40 ℃ * The collected effluent was evaporated to dryness, then made up to 1 mL with acetonitrile-tetrahydrofuran (9: 1) solution for HPLC analysis.

4 Analysis conditions

Column: Diamonsil C18 (2) 250 × 4.6 mm, 5 μm (Cat. #: 99603)

Flow rate: 1.0 mL / min

Detector: * Excitation wavelength: 370 nm Emission wavelength: 406 nm

Column temperature: 30 ℃

Injection volume: 10 μL

Mobile phase: acetonitrile: water = 97: 3

5 Add recycling results

5.1 Benzene (a) pyrene addition recovery results in food

Target compound matrix addition level (μg / kg) recovery rate (%)

Benzo (α) pyrene seasoning package 2.592.52

Instant noodles 1.094.05

5.2 Liquid chromatogram of benzo (a) pyrene (addition level 2.5 ng / g) in seasoning package

Detection solution of benzopyrene in instant noodles

5.3 Liquid chromatogram of benzo (a) pyrene (added level 1.0 ng / g) in instant noodle

Detection solution of benzopyrene in instant noodles

Product information related to the determination of benzopyrene in instant noodles

Article number name specification

Sample preparation

65351 Benzene pyrene detection special column ProElut BaP 22 g / 60 mL 10 / pk

24435812 Tube anti-cross contamination vacuum SPE extraction device 12

48031,3,6mL column and tube universal connector 15 / pk

4806 Cork (control flow) 15 / pk

99011 Vacuum / positive pressure dual-purpose pump, oil-free 1 / pk

99013 suction filter bottle set

(Including silicone rubber tube 2 meters, 2L suction filter bottle and rubber stopper) 1 / pk

1095 stainless steel dispensing needle 50 / PK

37177 Syringe Filter Nylon 13 mm, 0.22 μm 100 / pk

37180 syringe filter Nylon 13 mm, 0.45 μm 100 / pk

Chromatography column and guard column

99603 reversed phase high performance liquid chromatography column

Diamonsil C18 (2) 250 × 4.6mm, 5μm

6201EasyGuard C18 guard column 10 × 4.0mm 1 / pk

2 column cores + 1 column sleeve

Standard

12-N-11164-10MG Benzo (a) pyrene [50-32-8] 10 mg

HPLC solvent? Buffer salt? Ion pair reagent

50101 Acetonitrile HPLC grade 4 L

50115 n-hexane HPLC grade 4 L

50113 Tetrahydrofuran HPLC grade 4 L

General chromatography products

52401B bottle rack / blue 50 holes

52401A bottle rack / white 50 holes

5323 vial (brown / thread) 2 mL, 100 / pk

5325 sample bottle cap / with pad (already assembled) 100 / pk

H80465HPLC syringe 25 μL

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