Food contact materials - Polymer materials - Determination of bisphenol A in food sips - High performance liquid chromatography

Food contact materials - Polymer food simulants HPLC bisphenol A,

1 Scope

This standard specifies the method for determination of bisphenol A in food simulants.

This standard applies to the determination of bisphenol A in food simulant water, 3% acetic acid solution, 10% ethanol solution and olive oil.

2 normative references

The terms in the following documents become the terms of this standard by reference to this standard. All dated references, followed by all

Modifications (not including errata content) or revisions do not apply to this standard. However, parties to agreements based on this standard are encouraged to study whether the latest versions of these documents are available. For undated references, the latest edition applies to this standard.

SN/T 2280 food contact materials! Restricted substances in plastics! Specific migration test methods and content measurements for food and food simulants

Guidelines for the selection of exposure conditions for food simulants

3 method guide

After the water-based food simulated soaking liquid filtration membrane, it is determined by liquid chromatography; the olive oil simulated soaking liquid is extracted with methanol-water solution, and the extract is extracted.

It was filtered and measured by a liquid chromatograph.

4 reagents and materials

Unless otherwise specified, the reagents used were of analytical grade and the water was deionized water.

4.1 methanol

4.2 absolute ethanol

4.3 glacial acetic acid

4.4 methanol-water solution (1+1); measure 200ml of methanol (4.1) in a 1000ml beaker, add 200ml of water, mix

4.5 Refined olive oil

4.6 Bisphenol A standard material (Bisphenol A, CAS number: 105-60-2): purity ≥99%

4.7 Bisphenol A standard stock solution: Accurately weigh 50.0mg bisphenol A standard material (4.6) in a 100ml volumetric flask, add a small amount of methanol (4.1) to dissolve, and then dilute to the mark with methanol.

4.9 Aqueous simulated liquid medium: draw appropriate amount of bisphenol A standard stock solution (4.7), use water without test substance, 3% acetic acid solution, acetic acid solution, 10% B

The aqueous alcohol solution is formulated into standard working solutions of different concentrations.

4.9 Olive oil extract medium: Treat olive oil containing no test substance according to 7.1.2, and dilute the appropriate amount of bisphenol A standard with the obtained extract.

The stock solution (4.7) is formulated into standard working fluids of different concentrations.

5 Instruments and equipment

5.1 Liquid Chromatograph: equipped with a UV detector

GE-200 High Performance Liquid Chromatograph, GE-200 UV Detector, GE-200 High Efficiency Infusion Pump

5.2 Centrifuge: 5000r/min

6 sample preparation and preservation

6.1 Preparation of samples

The type, selection and migration conditions of the migration test soaking liquid are performed according to SN/T 2280.

7 Determination steps

7.1 Treatment of samples

7.1.1 Water-based simulated soaking solution

The water obtained by the migration test, the 3% acetic acid solution, and the 10% ethanol soaking solution were filtered through a 0.45 um filter, and analyzed by liquid chromatography.

7.1.2 Olive oil simulation soaking solution

Accurately weigh 1.00g of olive oil soaking solution, add 3.00ml of n-hexane, mix well, then add 2.0ml methanol-water solution (4.4), shake 10mlin and then centrifuge at 3000/min for 10min to take methanol-water solution layer through 0.45um filter Filtration, to be analyzed by liquid chromatography

7.2 Determination

7.2.1 Liquid chromatography conditions

Column: Vertex C18 250*4.5mm , 5um , or equivalent imported liquid chromatography column

Detection wavelength: 280nm

Mobile phase: methanol + water (3+1)

Flow rate: 0.8ml/min

Injection volume: 10ul

7.2.2 Chromatographic determination

The response values ​​of bisphenol A in the standard working solution and the sample to be tested should be within the linear range of the instrument. If the content of the solution to be tested exceeds the linear range, it should be diluted appropriately and then measured. For standard working solution and sample volume. Injection measurement. See the chromatogram of bisphenol A standard solution.

Appendix A. Recovery Data See Appendix B

7.2.3 Blank test

The food simulating liquid which was not subjected to the migration test was carried out as described above.

7.3 Calculation of results

The bisphenol A content in the sample is calculated according to formula (1):

X=C*A*V/AS*m

X---the content of bisphenol A in the sample, in milligrams per liter (mg/l)

C---concentration of standard working solution in bisphenol A, in milligrams per milliliter (ug/ml)

Peak area of ​​A---bisphenol A-like solution

AS---peak area of ​​bisphenol A-like quasi-working solution

V---the final volume of the sample solution, in milliliters (ml)

m---the volume of the sample in grams (g)

Note: When the mimetic is olive oil, the bisphenol A content is in milligrams per kilogram (mg/kg).

The method has the lower limit of 0.5mg/kg for the determination of the water-based food simulated soaking solution with a lower limit of 0.1mg/lL olive oil simulated soaking solution.

Appendix A of this standard, Appendix B "is an informative appendix"

This standard is proposed and under the jurisdiction of the National Certification and Accreditation Administration."

This standard was drafted by the People's Republic of China Shandong Entry-Exit Inspection and Quarantine Bureau"

The main drafters of this standard #孙忠松!王境堂!李杰!王建华!王俊!蔡发"

This standard is the first industry standard for entry-exit inspection and quarantine.

SN/T2282—2009