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GB 31604.35-2016National food safety standard - Food contact materials and products - Determination of caprolactam and migration quantity (English PDF)

食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定

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Issued by

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

Level / Type

National · Mandatory

Issue date

October 19, 2016

Implementation date

April 19, 2017

Scope

GB 31604.35-2016 is the English-translated version of 食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定.

GB 31604.35-2016 — This standard specifies the method for the determination of perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOAA) in food contact materials and products by tandem mass spectrometry.

This standard is applicable to the determination of PFOS and PFOA in food contact materials and products such as carton, rubber, polyethylene, plastics, resin, non-stick pan coating and so on.

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Document preview — GB 31604.35-2016

National Standard of the People's Republic of China

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

Contents

  • Foreword .3
  • 1 Scope ..4
  • 2 Principle..4
  • 3 Reagents and materials ..4
  • 4 Instruments and equipment .6
  • 5 Analytical steps .7
  • 6 Expression of the analytic result ..9
  • 7 Precision.10
  • 8 Others ..10
  • Appendix A Chromatogram .11

Foreword

This standard replaces GB/T 23243-2009 "Determination of perfluorooctane

sulfonates (PFOS) in the food packaging material - High performance liquid

chromatography-tandem mass spectrometry".

The main technical differences of this standard in comparison with GB/T 23243-

2009 are as follows.

- Changed the name of the standard to read "National Food Safety Standard

- Food contact materials and products - Determination of perfluorooctane

sulfonate (PFOS) and perfluoro caprylic acid (PFOA)";

- Added scope of application of the standard;

- Added the content of determination object PFOA;

- Added the method of sample preparation;

- Added the purification step. Use the weak anion exchange solid phase

extraction column to purify;

- Increased the sensitivity of the determination method.

National Food Safety Standard -

Food contact materials and products -

Determination of perfluorooctane sulfonate (PFOS) and

perfluoro caprylic acid (PFOA)

1 Scope

This standard specifies the method for the determination of perfluorooctane

sulfonate (PFOS) and perfluorooctanoic acid (PFOAA) in food contact materials

and products by tandem mass spectrometry.

This standard is applicable to the determination of PFOS and PFOA in food

contact materials and products such as carton, rubber, polyethylene, plastics,

resin, non-stick pan coating and so on.

2 Principle

PFOS and PFOA in food contact materials and products were extracted by

methanol to accelerate solvent extraction, purified by weak anion exchange

solid-phase extraction column, separated by liquid chromatography, ionized by

electrospray ionization, determined by multi-reaction monitoring mode and

quantified by Isotopic internal standard quantity.

3 Reagents and materials

Unless otherwise stated, the reagents used in this method shall be analytical

pure. The water shall be the primary water specified in GB/T 6682.

Note. All organic solvents and materials used in this standard shall be blank tested before using. If the

background value is higher than the quantitative limit, the organic solvent shall be re-steamed. Replace

the test material until the background value is below the limit of quantification.

3.1 Reagents

3.1.1 Methanol (CH3OH). Chromatographic purity.
3.1.2 Acetonitrile (CH3CN). Chromatographic purity.

5 Analytical steps

5.1 Sample preparation

For plastics, silica gel sample. cut to size below 5mm×5mm; then grind into

powder by liquid nitrogen frozen grinder. For resin. smash then grind into

powder with liquid nitrogen frozen grinder. For coated sample. scrape with knife,

then grind into powder by liquid nitrogen frozen grinder. For cardboard box and

polyethylene sample. use scissors to cut to 1cm×1cm.

5.2 Extraction and purification

5.2.1 Extraction

Weigh 1g (accurate to 0.01g) of sample and put it into an accelerated solvent

extraction pool. The extraction solvent is methanol. The volume of extraction

solvent is 60% the volume of the sample pool. The extraction temperature shall

be 110°C. The heating time shall be 5 min. Balance for 5 min. Repeat twice.

Place the extraction solution at room temperature. Dry with nitrogen-blowing to

about 0.5 mL. Add 10mL of water and mix for purification.

5.2.2 Purification

Activate and balance the WAX solid phase extraction column with 4 mL of

methanol animation, 4 mL of methanol and 4 mL of water in turn. Then transfer

the above solution to the solid phase extraction column. Add 4mL of 25mmol/L

ammonium acetate buffer solution to rinse-wash. Add 4 mL of 0.1% ammonia

methanol to elute. Collect the eluent and dry by nitrogen at 40°C. Re-dissolve

by 1 mL of methanol, then pour through.22µm microporous membrane. Analyze

by LC- MS/MS.

5.3 Reference conditions for liquid chromatography

5.3.1 Chromatographic column. C18, column length is 150mm, inner diameter

is 2.1mm, particle size is 3µm, or the column with equivalent performance.

5.3.2 Column temperature. 40 °C.
5.3.3 Sample volume. 10µL.
5.3.4 Mobile phase. 5 mmol/L ammonium acetate. acetonitrile. For gradient

elution conditions, see Table 1.

5.3.5 Flow rate. 0.2 mL/min.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 11 pages — is available in the English PDF.

Referenced standards

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