GB 31604.55-2023 National food safety standard - Food contact materials and products - Determination of migration of isothiazolinone compounds (English Version)
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard -
Food contact materials and articles -
Determination of isothiazolinone migration
1 Scope
This standard specifies the determination method of the migration of 1,2-Benzisothiazoline-3(2H)-one, 2-methyl-3 (2H)-isothiazolinone and 5-chloro-2-methyl-2H-isothiazolin-3-one in food contact materials and articles.
This standard is applicable to the determination of migration of 1,2-Benzisothiazoline-3(2H)-one, 2-methyl-3 (2H)-isothiazolinone and 5-chloro-2-methyl-2H-isothiazolin-3-one in food contact plastics, coatings and coating layers, rubber, paper and paperboard as well as food contact materials and articles using inks or adhesives.
Method I High performance liquid chromatography
2 Principle
The food contact materials and articles shall be subjected to testing using high performance liquid chromatography after migration test according to GB 31604.1 and GB 5009.156. Food simulants of 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50% (volume fraction) ethanol and chemical substitute solvent of 95% (volume fraction) ethanol soaking solution are filtered and directly injected; fatty food simulants and chemical substitute solvent of isooctane soaking solution are extracted by methanol-aqueous solution and then the water layer thereof is filtered for injection. An ultraviolet detector or diode array detector is used for detection, and peak area is quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents adopted for this method are chromatographically pure, and the water is Class-I water specified in GB/T 6682.
3.1 Reagents
3.1.1 Acid, alcoholic and fatty food simulants and chemical substitute solvents: the reagents used are in accordance with the requirements of GB 5009.156.
3.1.2 Methanol (CH4O).
3.1.3 Tetrahydrofuran (C4H8O).
3.1.4 n-hexane (C6H14).
3.2 Preparation of reagents
3.2.1 Acidic and ethanol-containing food simulants and chemical substitute solvents: prepared according to GB 5009.156.
3.2.2 Methanol solution: take 50 mL of methanol and 50 mL of water and mix well.
3.3 Standard
3.3.1 1,2-Benzisothiazoline-3(2H)-one(C7H5NOS, CAS No.: 2634-33-5): purity ≥95%, or a nationally recognized and certified standard.
3.3.2 2-Methyl-4-Isothiazolin-3-one (C4H5NOS, CAS No.: 2682-20-4): purity ≥95%, or a nationally recognized and certified standard.
3.3.3 5-Chloro-2-methyl-4-isothiazolin-3-one (C4H4ClNOS, CAS No.: 26172-55-4): purity ≥95%, or a nationally recognized and certified standard.
3.4 Preparation of standard solution
3.4.1 Isothiazolinone standard stock solution (1,000 mg/L in methanol): accurately weigh 25 mg (accurate to 0.1 mg) of each standard of 3 isothiazolinone standards, dissolve them in methanol, transfer the solution into a 25 mL brown volumetric flask, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass bottle and store it at 4°C in a refrigerator for 6 months.
3.4.2 Isothiazolinone standard intermediate solution A (100 mg/L in methanol): accurately pipette 0.5 mL each of the isothiazolinone standard stock solutions respectively, put them into a 10 mL brown volumetric flask respectively, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.3 Isothiazolinone standard intermediate solution B (10 mg/L in methanol): accurately pipette 1 mL isothiazolinone standard intermediate solution A into 10 mL brown volumetric flask, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.4 Isothiazolinone standard intermediate solution C (100 mg/L in tetrahydrofuran): accurately pipette 1 mL of three isothiazolinone standard stock solutions into a 10 mL brown volumetric flask, and dilute with tetrahydrofuran to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.5 Isothiazolinone standard intermediate solution D (10 mg/L in tetrahydrofuran): accurately transfer 1 mL isothiazolinone standard intermediate solution C in 10 mL brown volumetric flask, dilute with tetrahydrofuran to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
1 Scope
2 Principle
3 Reagents and materials
4 Apparatuses
5 Analytical procedures
6 Expression of analysis results
7 Precision
8 Others
9 Principle
10 Reagents and materials
11 Apparatuses
12 Analytical procedures
13 Expression of analysis results
14 Precision
Annex A High performance liquid chromatograms of three isothiazolinones
Annex B Mass spectrometry reference conditions
Annex C Total ion chromatogram (TIC) and mass spectrogram of three isothiazolinones by liquid chromatography-tandem mass spectrometry
Standard
GB 31604.55-2023 National food safety standard - Food contact materials and products - Determination of migration of isothiazolinone compounds (English Version)
Standard No.
GB 31604.55-2023
Status
valid
Language
English
File Format
PDF
Word Count
8500 words
Price(USD)
255.0
Implemented on
2024-9-6
Delivery
via email in 1 business day
Detail of GB 31604.55-2023
Standard No.
GB 31604.55-2023
English Name
National food safety standard - Food contact materials and products - Determination of migration of isothiazolinone compounds
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard -
Food contact materials and articles -
Determination of isothiazolinone migration
1 Scope
This standard specifies the determination method of the migration of 1,2-Benzisothiazoline-3(2H)-one, 2-methyl-3 (2H)-isothiazolinone and 5-chloro-2-methyl-2H-isothiazolin-3-one in food contact materials and articles.
This standard is applicable to the determination of migration of 1,2-Benzisothiazoline-3(2H)-one, 2-methyl-3 (2H)-isothiazolinone and 5-chloro-2-methyl-2H-isothiazolin-3-one in food contact plastics, coatings and coating layers, rubber, paper and paperboard as well as food contact materials and articles using inks or adhesives.
Method I High performance liquid chromatography
2 Principle
The food contact materials and articles shall be subjected to testing using high performance liquid chromatography after migration test according to GB 31604.1 and GB 5009.156. Food simulants of 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50% (volume fraction) ethanol and chemical substitute solvent of 95% (volume fraction) ethanol soaking solution are filtered and directly injected; fatty food simulants and chemical substitute solvent of isooctane soaking solution are extracted by methanol-aqueous solution and then the water layer thereof is filtered for injection. An ultraviolet detector or diode array detector is used for detection, and peak area is quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents adopted for this method are chromatographically pure, and the water is Class-I water specified in GB/T 6682.
3.1 Reagents
3.1.1 Acid, alcoholic and fatty food simulants and chemical substitute solvents: the reagents used are in accordance with the requirements of GB 5009.156.
3.1.2 Methanol (CH4O).
3.1.3 Tetrahydrofuran (C4H8O).
3.1.4 n-hexane (C6H14).
3.2 Preparation of reagents
3.2.1 Acidic and ethanol-containing food simulants and chemical substitute solvents: prepared according to GB 5009.156.
3.2.2 Methanol solution: take 50 mL of methanol and 50 mL of water and mix well.
3.3 Standard
3.3.1 1,2-Benzisothiazoline-3(2H)-one(C7H5NOS, CAS No.: 2634-33-5): purity ≥95%, or a nationally recognized and certified standard.
3.3.2 2-Methyl-4-Isothiazolin-3-one (C4H5NOS, CAS No.: 2682-20-4): purity ≥95%, or a nationally recognized and certified standard.
3.3.3 5-Chloro-2-methyl-4-isothiazolin-3-one (C4H4ClNOS, CAS No.: 26172-55-4): purity ≥95%, or a nationally recognized and certified standard.
3.4 Preparation of standard solution
3.4.1 Isothiazolinone standard stock solution (1,000 mg/L in methanol): accurately weigh 25 mg (accurate to 0.1 mg) of each standard of 3 isothiazolinone standards, dissolve them in methanol, transfer the solution into a 25 mL brown volumetric flask, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass bottle and store it at 4°C in a refrigerator for 6 months.
3.4.2 Isothiazolinone standard intermediate solution A (100 mg/L in methanol): accurately pipette 0.5 mL each of the isothiazolinone standard stock solutions respectively, put them into a 10 mL brown volumetric flask respectively, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.3 Isothiazolinone standard intermediate solution B (10 mg/L in methanol): accurately pipette 1 mL isothiazolinone standard intermediate solution A into 10 mL brown volumetric flask, dilute with methanol to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.4 Isothiazolinone standard intermediate solution C (100 mg/L in tetrahydrofuran): accurately pipette 1 mL of three isothiazolinone standard stock solutions into a 10 mL brown volumetric flask, and dilute with tetrahydrofuran to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
3.4.5 Isothiazolinone standard intermediate solution D (10 mg/L in tetrahydrofuran): accurately transfer 1 mL isothiazolinone standard intermediate solution C in 10 mL brown volumetric flask, dilute with tetrahydrofuran to the scale, and shake well. Transfer the solution to a brown glass container and store it at 4°C away from light in a refrigerator for 3 months.
Contents of GB 31604.55-2023
1 Scope
2 Principle
3 Reagents and materials
4 Apparatuses
5 Analytical procedures
6 Expression of analysis results
7 Precision
8 Others
9 Principle
10 Reagents and materials
11 Apparatuses
12 Analytical procedures
13 Expression of analysis results
14 Precision
Annex A High performance liquid chromatograms of three isothiazolinones
Annex B Mass spectrometry reference conditions
Annex C Total ion chromatogram (TIC) and mass spectrogram of three isothiazolinones by liquid chromatography-tandem mass spectrometry
