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SN/T 5155-2019Test methods for food contact materials -- Polymer - Determination of crotonic acid in food sin ulants -- High performance liquid chromatography (English PDF)

食品接触材料检测方法高分子材料食品模拟物中巴豆酸含量的测定高效液相色谱法

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Issued by

General Administration of Customs

Level / Type

National · Recommended

Issue date

October 25, 2019

Implementation date

May 1, 2020

Scope

SN/T 5155-2019 is the English-translated version of 食品接触材料检测方法高分子材料食品模拟物中巴豆酸含量的测定高效液相色谱法.

SN/T 5155-2019 — This standard specifies the HPLC method for the determination of crotonic acid in food simulants.

This standard applies to 3% (mass concentration) acetic acid, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol solution, 20% (volume fraction) Number) Determination of crotonic acid in six food simulants, ethanol solution, 50% (volume fraction) ethanol solution and olive oil.

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Document preview — SN/T 5155-2019

National Standard of the People's Republic of China

Classification: C 53

Issued by: General Administration of Customs

Foreword
1 Scope
2 Normative references
3 Method summary
4 Reagents and materials
5 Instruments and equipment
6 Preparation of test solution
6.1 Preparation of standard working solution
6.2 Preparation of food simulant test solution
6.3 Preparation of blank test solution
7 Quantitative determination
7.1 Instrument reference conditions
7.2 Draw a standard working curve
7.3 Test solution determination
8 Calculation of results
8.2 Calculation of crotonic acid concentration in olive oil food simulants
9 Low limit of determination
10 Repeatability

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This standard is proposed and managed by the General Administration of Customs of the People's Republic of China.

This standard was drafted. Tianjin Customs of the People's Republic of China, Ningbo Customs of the People's Republic of China.

1 Scope

This standard specifies the HPLC method for the determination of crotonic acid in food simulants.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies file. For undated references, the latest version (including all amendments) applies to this document.

GB/T 6682 Analytical laboratory water specifications and test methods GB/T 232966.1 Food contact materials. Restricted substances in plastics. Specific migration of substances in plastics to food and food simulants.

Guidelines for testing and content determination methods and selection of food simulant exposure conditions GB 31604.1 National Food Safety Standard General Rules for Migration Test of Food Contact Materials and Products

3 Method summary

After the sample is immersed in the food simulant, a certain amount of food simulant test solution is taken (of which the olive oil test solution needs ultrasonic-assisted liquid-liquid extraction), the content of crotonic acid was determined by high performance liquid chromatography and quantified by external standard method.

4 Reagents and materials

Unless otherwise specified, the reagents used are of analytical grade and the water is secondary water as specified in GB/T 6682.

4.1 Glacial acetic acid.

4.2 Anhydrous ethanol.

4.3 Methanol. chromatographically pure.

4.4 Formic acid. chromatographically pure.

4.5 3% (mass-volume concentration) acetic acid solution. Weigh 30.0g (accurate to 0.1g) glacial acetic acid (4.1), dilute with water and transfer to 1L in a volumetric flask, make up to volume with water.

4.6 4% (volume fraction) acetic acid solution. Measure 40mL of glacial acetic acid (4.1) in a 1L volumetric flask, and make up to volume with water.

4.7 10% (volume fraction) ethanol solution. Measure 100mL of absolute ethanol (4.2) in a 1L volumetric flask, and make up to volume with water.

4.8 20% (volume fraction) ethanol solution. Measure.200mL of absolute ethanol (4.2) into a 1L volumetric flask, and make up to volume with water.

4.9 50% (volume fraction) ethanol solution. Measure 500mL of absolute ethanol (4.2) in a 1L volumetric flask, and make up to volume with water.

4.10 Commercially available olive oil.

4.11 Crotonic acid standard, CASN O... [3724-65-0], purity >=99.5%.

SN/T 5155-2019

4.12 Crotonic acid standard stock solution. Accurately weigh crotonic acid (4.11) 0.05g (accurate to 0.1mg), use methanol to dissolve and transfer to in a 500mL brown volumetric flask, make up to volume with methanol (4.3) and mix thoroughly to obtain a standard stock solution with a concentration of 100mg/L, 4 °C Save it for future use. Shelf life is 1 month.

4.13 Microporous membrane. water phase and organic phase, pore size 0.2 µm.

5 Instruments and equipment

5.1 High Performance Liquid Chromatograph (HPLC). Equipped with UV detector.

5.2 Ultrasonic extraction instrument.

5.3 Test tube with stopper. 10mL.

5.4 Syringe. 2mL.

5.5 Micropipette. 10 µL, 100 µL, 1000 µL. 5.6 Analytical balance. Sensitivity of 0.1mg and 0.01g.

6 Preparation of test solution

6.1 Preparation of standard working solution

6.1.1 Water-based food simulant standard working solution

Use micropipettes (5.5) to accurately measure 50 µL, 80 µL, 100 µL, 300 µL, 500 µL, 800 µL, 1000 µL of crotonic acid standard stock solution (4.12) in 7 10 mL volumetric flasks, and use migration tests respectively. Volume of water-based food simulant selected in the shaker, shake the back chamber evenly After standing at room temperature for 24 hours, the concentrations of crotonic acid in the corresponding media were 0.5 mg/L, 0.8 mg/L, 1.0 mg/L, 3.0 mg/L, Standard working solutions of 5.0 mg/L, 8.0 mg/L and 10 mg/L.

6.1.2 Standard working solution of olive oil

Using a syringe (5.4), accurately weigh 2g (accurate to 0.01g) olive oil into 6 test tubes (5.3) with stoppers, and use a micropipette (5.5) Transfer 20 µL, 40 µL, 100 µL, 160 µL,.200 µL, 400 µL of crotonic acid standard stock solution (4.12) to stoppered test tubes (5.3) to obtain concentrations of 1 mg/kg and 2 mg respectively/Kg, 5mg/kg, 8mg/kg, 10mg/kg, 20mg/kg standard working solution. 4mL of methanol (4.3) was added to each test tube. After ultrasonic extraction at 60 ° C for 60min, the layers were left to separate and aspirated with a syringe (5.4).

Take a methanol solution to obtain a standard working solution of crotonic acid with different concentrations. After filtering through a 0.2 µm filter membrane (4.13), use it for liquid chromatography determination.

6.2 Preparation of food simulant test solution

6.2.1 Sample pretreatment

Wash the sample with detergent, rinse it with tap water, rinse it three times with ultrapure water, dry it, and set aside.

6.2.2 Migration experiment

The migration test shall be carried out in accordance with GB 31604.1 or GB/T 23296.1.

6.2.3 Treatment of food simulant test solution

For a water-based food simulant test solution, take an appropriate amount of the simulant solution and filter it through a 0.2 µm filter membrane (4.13) for detection by a liquid chromatograph. For olive oil test solution, weigh 2.0g (accurate to 0.01g) olive oil test solution into a 10mL stoppered test tube (5.3), add 4mL of methanol (4.4), After ultrasonic extraction at 60 ° C for 60 min, the layers were left to stand, the methanol solution was aspirated with a syringe (5.4), filtered through a 0.2 µm filter membrane (4.13), and then determined by liquid chromatography.

SN/T 5155-2019

6.3 Preparation of blank test solution

Dispose of food simulants that are not in contact with food contact materials in accordance with 6.2.

7 Quantitative determination

7.1 Instrument reference conditions

Because the test results depend on the instrument used, it is not possible to give general parameters for chromatographic analysis. Set the parameters to ensure the chromatogram the measured components can be effectively separated from other components during the determination. The parameters given below prove to be feasible.

7.1.1 Chromatographic column. C18 column, with a column length of 150 mm, an inner diameter of 2.1 mm, and a particle size of 5.0 µm or equivalent 7.1.2 Mobile phase. water (0.17% formic acid solution). methanol (90.10, volume ratio).

7.1.3 Flow rate. 1.0mL/min.

7.1.4 Column temperature. 30 ° C.

7.1.5 Injection volume. 10 µL. 7.1.6 Detection wavelength. 210nm.

7.2 Draw a standard working curve

Test the standard working solution (6.1) according to the measurement conditions listed in 7.1. Crotonic acid concentration in food simulant standard working solution is the abscissa, the unit is expressed in milligrams per kilogram or milligram per liter (mg/kg or mg/L).

Draw a standard working curve. The chromatogram of standard solution of crotonic acid is shown in Appendix A, Figure A. 1.

7.3 Test solution determination

The blank test solution (6.3) and food simulant test solution (6.2) were sampled in equal volumes according to the steps of 6.2 to 7.3.

8 Calculation of results

8.1 Calculation of crotonic acid concentration in water-based food simulants.

The content of crotonic acid in a water-based food simulation can be calculated directly by a computer workstation or by formula (1).

X = (A-A0) × As (1)

In the formula.

X --- crotonic acid concentration in food simulants, the unit is milligram per liter of food simulant (mg/L);

A --- the peak area of crotonic acid in the test solution;

A0 --- the peak area of crotonic acid in the blank;

As --- the peak area of crotonic acid in the standard working solution;

--- The concentration of crotonic acid in the standard working solution, the unit is milligram per liter (mg/L).

8.2 Calculation of crotonic acid concentration in olive oil food simulants

The content of crotonic acid in olive food simulants can be calculated directly by a computer workstation, or it can be calculated by formula (2).

In the formula.

X --- crotonic acid concentration in food simulants, the unit is milligram per kilogram of food simulant (mg/kg) SN/T 5155-2019 A --- the peak area of crotonic acid in the test solution;

A0 --- the peak area of crotonic acid in the blank;

As --- the peak area of crotonic acid in the standard working solution;

--- The concentration of crotonic acid in the standard working solution, the unit is milligram per kilogram (mg/kg);

The calculation results are expressed as the arithmetic mean of the parallel determinations, with three significant digits retained.

9 Low limit of determination

The lower limits for the determination of crotonic acid in different mimics are shown in Table 1 below.

Table 1 Lower limit of determination of crotonic acid in water-based food simulants and olive oil

Food simulation

Type

10% (volume

Fraction) ethanol

3% (quality

Concentration) acetic acid 4% (volume Fractions) Acetic acid 20% (volume Fraction) ethanol 50% (volume Fractions) Ethanol and olive oil Low limit of determination 0.5mg/L 0.5mg/L 0.5mg/L 0.5mg/L 0.5mg/L 1.0mg/kg

10 Repeatability

The absolute difference between the two independent determination results obtained under repeatable conditions shall not exceed 10% of the arithmetic mean.

SN/T 5155-2019

Appendix A

(Informative appendix) Chromatogram of standard solution of crotonic acid in food simulants

Figure A. 1 Chromatogram of standard solution of crotonic acid in food simulants

SN/T 5155-2019

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 6 pages — is available in the English PDF.

Referenced standards

Normative references

GB/T 232966.1

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