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GB 31604.15-2016National food safety standard - Food contact materials and articles - Determination of migration of 2,4,6-triamino-1,3,5-triazine (melamine) (English PDF)

食品安全国家标准 食品接触材料及制品 2,4,6-三氨基-1,3,5-三嗪(三聚氰胺)迁移量的测定

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Issued by

National Health and Family Planning Commission of the People's Republic of China

Level / Type

National · Mandatory

Issue date

October 19, 2016

Implementation date

April 19, 2017

Scope

GB 31604.15-2016 is the English-translated version of 食品安全国家标准 食品接触材料及制品 2,4,6-三氨基-1,3,5-三嗪(三聚氰胺)迁移量的测定.

GB 31604.15-2016 — This Standard specifies the method for the determination of migration of melamine in food contact materials and articles (melamine-formaldehyde resins and their moldings).

This Standard applies to the high performance liquid chromatography for the determination of migration of melamine in food contact materials and articles (melamine-formaldehyde resins and their moldings).

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Document preview — GB 31604.15-2016

National Standard of the People's Republic of China

Issued by: National Health and Family Planning Commission of the People's Republic of China

Contents

  • Foreword .3
  • 1 Scope ..4
  • 2 Principle .4
  • 3 Reagents and materials ..4
  • 4 Apparatus .6
  • 5 Analytical procedures .7
  • 6 Expression of analysis results ..8
  • 7 Precision .8
  • 8 Others .9
  • Annex A Chromatograms of melamine in food simulant test solutions ..10

Foreword

This Standard replaces GB/T 23296.15, Food contact materials - Polymer -

Determination of 2 4 6-triamino-1 3 5-triazine(melamine)in food simulants - High

performance liquid chromatography.

Compared with GB/T 23296.15-2009, the major changes of this Standard are as

follows.

-- the standard name is changed into "National food safety standard - Food contact

materials and articles - Determination of migration of 2,4,6-triamino-1,3,5-triazine

(melamine)".

National food safety standard –

Food contact materials and articles - Determination of

migration of 2,4,6-triamino-1,3,5-triazine (melamine)

1 Scope

This Standard specifies the method for the determination of migration of melamine in

food contact materials and articles (melamine-formaldehyde resins and their moldings).

This Standard applies to the high performance liquid chromatography for the

determination of migration of melamine in food contact materials and articles

(melamine-formaldehyde resins and their moldings).

2 Principle

Make food contact materials and articles (melamine-formaldehyde resins and their

moldings) in contact with food simulants; carry out migration test under certain soaking

conditions; use the high performance liquid chromatography to test the test solution

obtained from soaking treatment; and then convert into the specific migration of

melamine. Based on food categories, select the corresponding food simulants and

migration test conditions (time and temperature) in accordance with GB 31604.1.

When the food simulant includes water, acetic acid of 4% (volume fraction), ethyl

alcohol of 10%, 20% or 50%~95% (volume fraction), use the soak solution directly as

test solution. When the food simulant is vegetable oil, use the test solution obtained by

the extraction treatment of soak solution directly as sample; use the high performance

liquid chromatography to determine the content of melamine in test solution; determine

the soak solution volume and sample contact area for migration test in accordance

with GB 5009.156; and convert into the specific migration of melamine (release amount

of migrated substance).

3 Reagents and materials

Unless indicated otherwise, all reagents used for this method are analytically pure and

the water is grade one water specified in GB/T 6682. The use of plastic material shall

be avoided in test containers and transfer instruments.

3.1 Reagents

3.4.3 Preparation of food simulant standard working solution
3.4.3.1 Standard working solutions of water-based, acidic and alcoholic food

simulants

Accurately absorb 0 mL, 0.125 mL, 0.250 mL, 1.25 mL and 2.50 mL of melamine

standard intermediate solution (3.4.2) respectively to pour into a 25 mL volumetric flask;

and use water-based food simulant to add to scale. The concentrations of melamine

are respectively 0 mg/L, 0.500 mg/L, 1.00 mg/L, 5.00 mg/L and 10.0 mg/L. Use the

same method to prepare melamine standard working solutions of the same

concentration series using acidic and alcoholic food simulants respectively.

3.4.3.2 Standard working solutions of oil-based food simulants

Accurately weigh 5 g (accurate to 0.01 g) of oil-based food simulant (refined corn oil

or olive oil) to pour respectively into five 25 mL glass test tubes with a stopper; use an

adjustable pipette to transfer 0 µL, 25.0 µL, 50.0 µL, 250 µL and 500 µL of melamine

standard intermediate solution (3.4.2) respectively to a test tube; and obtain the

standard working solutions of oil-based food simulants. The concentrations of

melamine are respectively 0 mg/kg, 0.500 mg/kg, 1.00 mg/kg, 5.00 mg/kg and 10.00

mg/kg. Add 5.0 mL of isooctane to each test tube and mix up; add 5.0 mL of isopropyl

alcohol solution (3.2.4); place test tubes in a thermostatic water bath at 70°C for

ultrasonic extraction for 30 min; and then carry out centrifugal separation. Absorb 1

mL~2 mL of the lower layer of the aqueous solution; and pass through an organic

phase microporous membrane 0.22 µm to obtain test solutions, which are used for the

high performance liquid chromatograph to carry out determination.

3.5 Material

Organic phase microporous membrane. 0.22 µm.

4 Apparatus

4.1 High performance liquid chromatograph. equipped with an ultraviolet absorption

detector or luminous diode array detector.

4.2 Vortex oscillator.

4.3 Ultrasonic thermostatic water bath.

4.4 Centrifuge. rotational speed greater than 4 000 r/min.

4.5 Analytical balance. of sensitivities 0.000 1 g and 0.01 g.

......

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.

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