Circular No. 14/2010/TT-BYT Issuing National Technical Regulations on substances used to supplement zinc in food

CIRCULAR

Issuing National Technical Regulations on substances

to be used for zinc fortification in food

Pursuant to the Law on Standards and Technical Regulations dated June 29, 2006 and Decree No. 127/2007/NĐ-CP dated August 1, 2007 of the Government detailing the implementation of certain provisions of the Law on Standards and Technical Regulations;

Pursuant to the Ordinance on Food Safety dated August 7, 2003 and Decree No. 163/2004/NĐ-CP dated September 7, 2004 of the Government detailing the implementation of certain provisions of the Ordinance on Food Safety;

Pursuant to Decree No. 188/2007/NĐ-CP dated December 27, 2007 of the Government stipulating the functions, tasks, powers, and organizational structure of the Ministry of Health;

At the proposal of the Director of the Food Safety Agency, the Head of the Science and Training Department, and the Head of the Legal Affairs Department,

c) Enterprises may be granted permission for no more than one block out of the total three dual-frequency blocks (FDD) B

Article 1. 1. National Technical Regulation on Railway Traffic Signals, number QCVN 21:2025/BXD.

QCVN 3-1:2010/BYT - National Technical Regulation on substances to be used for zinc fortification in food.

Article 2. This Circular takes effect from January 1, 2011.

Article 3. The Director of the Food Safety Agency, Heads of units under the Ministry of Health, units directly under the Ministry of Health; Directors of Health Departments of provinces and centrally governed cities and relevant organizations and individuals are responsible for implementing this Circular./.
 

QCVN 3-1: 2010/BYT
NATIONAL TECHNICAL REGULATION
ON SUBSTANCES TO BE USED FOR ZINC FORTIFICATION IN FOOD
INTO FOOD
National technical regulation
on substances that may be added for zinc fortification in food

Preamble
QCVN 3-1: 2010/BYT was drafted by the National Technical Regulation Drafting Board on Nutrient-Fortified Foods, submitted for review by the Food Safety Agency, and issued pursuant to Circular No. 14/2010/TT-BYT dated May 20, 2010 of the Minister of Health.
1. Scope of Application
This National Technical Regulation (hereinafter referred to as the Regulation) sets forth technical requirements and quality and safety management requirements for substances used for zinc fortification in food.
2. Applicability
NATIONAL TECHNICAL REGULATION
ON SUBSTANCES TO BE USED FOR ZINC FORTIFICATION IN FOOD
INTO FOOD
National technical regulation
on substances that may be added for zinc fortification in food
This technical regulation sets out technical requirements, testing methods, sampling procedures; management requirements; responsibilities of organizations and individuals producing, trading, and importing cigarettes.
This Regulation applies to:
2.1. Organizations and individuals importing, exporting, producing, trading, and using substances for zinc fortification in food (hereinafter referred to as organizations and individuals).
2.2. Relevant state management agencies.
3. Explanation of Terms and Abbreviations
3.1. Substances for zinc fortification in food: These are substances actively added to food with the purpose of zinc fortification.
3.2. Food Chemical Codex 2008: A set of standards of the United States (applied in Canada, Australia, and New Zealand) for substances used in food (food additives, processing aids, nutrient supplements, etc.), published by the United States Pharmacopeia in its 6th edition in 2008.
3.3. CAS number (Chemical Abstracts Service): A registration number for chemicals of the American Chemical Society.
3.4. TS (test solution): Test solution.
3.5. R (Reagent): Reagent.
3.6. VS (Volumetric solution): Standard solution.
II. TECHNICAL REQUIREMENTS AND TESTING METHODS
1. Technical requirements and testing methods for substances for zinc fortification in food are specified in the appendices accompanying this Regulation as follows:
1.1. Appendix 1: Technical requirements and testing methods for zinc sulfate.
1.2. Appendix 2: Technical requirements and testing methods for zinc oxide.
2. The technical requirements stipulated in this Regulation shall be tested according to the Food Chemical Codex 2008, except for the testing methods specifically guided in this Regulation; equivalent testing methods may also be used.
3. Sampling shall be conducted in accordance with Circular No. 16/2009/TT-BKHCN dated June 2, 2009 of the Ministry of Science and Technology on guidelines for national inspection of the quality of goods circulating in the market and other relevant legal regulations.
III. MANAGEMENT PROVISIONS
1. Declaration of Compliance
1.1. Substances used for zinc fortification in food must be declared in compliance with the provisions of this Regulation.
1.2. The method, procedure, and formalities for declaring compliance shall be carried out in accordance with the regulations on certification of conformity, declaration of conformity, and issuance of certificates of conformity and declarations of conformity promulgated together with Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the Minister of Science and Technology and other relevant legal regulations.
2. Inspection of Substances for Zinc Fortification in Food
Quality and safety inspections of substances for zinc fortification in food must be carried out in accordance with the provisions of the law.
1. Organizations and individuals must declare compliance in accordance with the technical requirements of this Regulation, register their declaration of compliance with the Food Safety Agency, and ensure quality and safety in accordance with the contents of the declaration.
2. Organizations and individuals may only import, export, produce, trade, and use substances for zinc fortification in food after completing the registration of their declaration of compliance and ensuring quality, safety, and labeling in accordance with the provisions of the law.
1. The Food Safety Agency shall take the lead and coordinate with relevant functional agencies to guide the implementation and organization of enforcement of this Regulation.
2. Based on management requirements, the Food Safety Agency has the responsibility to propose the Ministry of Health to amend and supplement this Regulation.
3. In cases where international guidance on testing methods and legal provisions cited in this Regulation are amended, supplemented, or replaced, the new provisions shall apply.
TECHNICAL REQUIREMENTS AND TESTING METHODS FOR ZINC SULFATE
1. Definition
CAS number
Chemical formula
Molecular weight
2. Sensory characteristics
3. Function
4. Technical requirements
4.1. Qualitative analysis
Solubility
Zinc
Sulfate
4.2. Purity
Alkaline and alkaline earth metals
Cadmium
Lead
Mercury
Selenium
IV. RESPONSIBILITIES OF ORGANIZATIONS AND INDIVIDUALS
Zinc sulfate.
K
Monohydrate form: 7445-19-7.
Heptahydrate form: 7446-20-0.
use zinc supplements in food after completing the registration of the declaration
compliance and ensuring quality, safety, hygiene, and appropriate labeling in accordance with
legal regulations.
V. IMPLEMENTATION
1. Entrust the Food Safety Agency to lead and coordinate with relevant agencies to guide the implementation and organization of this Standard's execution.
2. Based on management requirements, the Food Safety Agency has the responsibility to propose amendments to this Standard to the Ministry of Health.
3. In cases where international guidance on testing methods and legal provisions cited in this Standard are revised, supplemented, or replaced, the new provisions shall be applied.
TECHNICAL REQUIREMENTS AND TESTING METHODS FOR ZINC SULFATE
1. Definition
CAS Number
Chemical Formula
Appendix 1
Molecular Weight
2. Sensory Characteristics
3. Function
Chemical name
4. Technical Requirements
4.1. Qualitative Analysis
Solubility
Zinc
Sulfate
4.2. Purity
Alkali and Alkaline Earth Metals
Cadmium
Lead
Mercury
Selenium
Zinc sulfate.
K
Monohydrate form: 7445-19-7.
Heptahydrate form: 7446-20-0.
Dissolve in a small cup in 10 ml distilled water. Add 1 ml
of 1/5 sulfuric acid solution and 1 ml of 1/25 potassium permanganate solution. Cover the cup mouth, boil for a few
seconds, then let it cool.
5.3. Quantitative Analysis - Test according to Food Chemical Codex 6 (Special Discussion on Limit Selenium Testing, Method I - Appendix III B). - Sample: 200 mg. - Sample: Weigh 175 mg of the monohydrate form or 300 mg
of the heptahydrate form. - Analysis: Dissolve the sample in 100 ml distilled water,
Monohydrate form: ZnSO4.H2O.
Heptahydrate form: ZnSO4.7H2O.
Monohydrate form: 179.45.
Heptahydrate form: 287.54.
Zinc sulfate preparation has a crystalline prism shape, transparent or small needle-shaped crystals, or granular, fine crystal powder form. The molecule may contain either 1 or 7 water molecules of hydration. The heptahydrate form may lose water in dry air at room temperature, while the monohydrate form loses water at 238°C. The solution turns acidic when tested with litmus paper.
Nutrient.
Monohydrate form dissolves in water but does not dissolve in alcohol. One gram of the heptahydrate form dissolves in 0.6 ml of water, approximately 2.5 ml of glycerin; it does not dissolve in alcohol.
There must be characteristic reactions of zinc.
There must be characteristic reactions of sulfate.
Not to exceed 0.5%.
Not to exceed 2.0 mg/kg.
Not to exceed 4.0 mg/kg.
Not to exceed 5.0 mg/kg.
Not to exceed 0.003%.
4.3. Quantitative analysis.
4.4. Acidity.
5. Testing methods.
5.1. Qualitative testing.
5.2. Purity.
Alkali and alkaline earth metals.
Monohydrate form: Not less than 98.0% and not more than 100.5% ZnSO4.H2O.
Heptahydrate form: Not less than 99.0% and not more than 108.7% ZnSO4.7H2O.
Sample solution in distilled water (50 mg/ml) must not have a pink color when methyl orange solution (TS) is added. Test according to Food Chemical Codex 6 (specific chapter on zinc identification, Appendix III A). - Sample solution: 50 mg/ml. - Test according to Food Chemical Codex 6 (specific chapter on sulfate identification, Appendix III A). - Sample solution: 50 mg/ml. - Sample: Weigh 2 g - Proceeding with test: Transfer the weighed sample into a 200 ml volumetric flask, dissolve the sample in about 150 ml distilled water. Precipitate all zinc by adding ammonium sulfide solution (TS). Dilute to volume with distilled water, shake well. Filter through dry filter paper, discard the initial filtrate portion, take the next 100 ml of filtrate. Add a few drops of sulfuric acid. Evaporate to dryness on a pre-weighed dish. Heat until constant weight. - Residue left must not exceed 5 mg. - Test according to Food Chemical Codex 6 (specific chapter on cadmium limit test, Appendix III B). - Test according to Food Chemical Codex 6 (specific chapter on lead limit test using amine pyrolidindithio carbamate APDC method - Appendix III). - Sample: 5 g. - Test according to Food Chemical Codex 6 (specific chapter on mercury limit test - Appendix III B).
Prepare the sample: Weigh 400 mg of the sample, place it in a small beaker, dissolve in 10 ml distilled water. Add 1 ml of 1/5 sulfuric acid solution and 1 ml of 1/25 potassium permanganate solution. Cover the beaker mouth, boil for a few seconds, let cool.
5.3. Quantitative analysis - Test according to Food Chemical Codex 6 (specific chapter on selenium limit test, Method I - Appendix III B). - Sample: 200 mg. - Sample: Weigh 175 mg of the monohydrate form or 300 mg of the heptahydrate form. - Analysis: Dissolve the sample in 100 ml distilled water, add 5 ml of ammonia-ammonium chloride buffer solution (TS) and add 0.1 ml of eriochrome black T solution (TS). Titrate with sodium EDTA 0.05M solution until the solution turns a clear blue color.
Each milliliter of sodium EDTA 0.05M solution is equivalent to 8.973 mg ZnSO4.H2O or 14.38 mg ZnSO4.7H2O.
Lead
Mercury
6. Packaging and storage Keep in sealed packaging without air.
Appendix 2
K
Monohydrate form: 7445-19-7.
Heptahydrate form: 7446-20-0.
FOR ZINC OXIDE
1. Definition
Zinc
Burn over fire
Loss of mass when heated
Alkalinity
Non-precipitating substances with sulfide
Zinc oxide
ZnO
Zinc oxide preparation has an amorphous white powder form, smooth. When exposed to air, it can slowly absorb carbon dioxide.
Insoluble in water, insoluble in alcohol; soluble in dilute acid solutions and strong alkali solutions.
When heated, the sample turns yellow, this yellow color will disappear when cooled.
Not to exceed 1.0%.
Meets requirements (described in the testing method section).
Not to exceed 3.0 mg/kg.
Not to exceed 10.0 mg/kg.
Not to exceed 0.5%.
4.3. Quantitative analysis The content of ZnO in the product after calcination must not be less than 99.0%.
Test according to Food Chemical Codex 6 (specific chapter on zinc qualitative test). - Sample solution: Dissolve the sample in 3N hydrochloric acid solution, add a little excess acid. - Test according to Food Chemical Codex 6. - Sample: 2 g. - Analysis: Calcine at 800°C ± 25°C until constant weight.
Weigh 2 g of the sample, disperse in 20 ml distilled water. Boil for 1 minute, filter the filtrate. Add 0.1 ml of phenolphthalein solution (TS) to the filtrate, the filtrate must not turn red.
Test according to Food Chemical Codex 6 (specific chapter on cadmium limit test). - Sample solution: Accurately weigh 5 g of the sample, place in a 50 ml volumetric flask, dissolve the sample in a minimum amount of hydrochloric acid (2:3) solution. Dilute to volume with distilled water, shake well. - Test according to Food Chemical Codex 6 (specific chapter on pyrolidindithio carbamate APDC). - Sample: 2 g - Sample: 2 g - Analysis: Place the sample in a 200 ml flask, dissolve the sample in 20 ml of glacial acetic acid (1:4) solution. Dilute to about 150 ml with distilled water, shake well. Precipitate all zinc with ammonium sulfide solution (TS), dilute to volume with distilled water. Filter through dry filter paper, discard the initial filtrate portion, then take 100 ml of filtrate. Add a few drops of sulfuric acid to the obtained filtrate. Evaporate to dryness on a water bath and in a pre-weighed dish. Heat the dish until all ammonium salt evaporates, then calcine at 800°C ± 25°C until constant weight and weigh. The residue weight must not exceed 5 mg.
5.3. Quantitative analysis - Sample: Weigh 1.5 g of freshly calcined product. - Analysis: Dissolve the sample and 2.5 g of ammonium chloride in 50 ml of 1N sulfuric acid, heat gently if necessary. When the sample is completely dissolved, add a few drops of methyl orange solution (TS) and titrate the excess sulfuric acid with sodium hydroxide solution.
add 5 ml of ammonium chloride buffer solution (TS)
and add 0.1 ml of eriochrome black T solution (TS). Titrate with 0.05M disodium EDTA solution until the
solution turns a clear blue color.
Each milliliter of 0.05M disodium EDTA solution is equivalent
Dissolve in a small cup in 10 ml distilled water. Add 1 ml
to 8.973 mg ZnSO4.H2O or 14.38 mg ZnSO4.7H2O.
6. Packaging and Storage Keep in sealed packaging without air exposure.
ANNEX 2
TECHNICAL REQUIREMENTS AND TESTING METHODS FOR ZINC OXIDE
1. Definition
Zinc
Burn over fire
Loss in weight when
heated
Alkalinity
Non-sulfide precipitates
Molecular Weight
Zinc oxide
ZnO
Chemical name
4. Technical Requirements
4.1. Qualitative Analysis
Solubility
Zinc
Sulfate
4.2. Purity
Alkali and Alkaline Earth Metals
Cadmium
Zinc oxide preparation is in white, fine amorphous powder form. When exposed to air, it may gradually absorb
carbon dioxide.
Selenium
Insoluble in water, insoluble in alcohol; soluble in
dilute acids and strong alkalis.
When heated, the sample turns yellow, and this yellow
K
Monohydrate form: 7445-19-7.
color will disappear upon cooling the sample.
Not more than 1.0%.
Meets the requirement (described in the testing method section).
seconds, then let it cool.
1314-13-2 
Not more than 3.0 mg/kg.
81,38 
Not more than 10.0 mg/kg.
Not more than 0.5%.
4.3. Quantitative Analysis The zinc oxide content in the preparation after heating must not be less than 99.0%.
Not to exceed 4.0 mg/kg.
Test according to the instructions in Food Chemical Codex 6
(Special Discussion on Qualitative Zinc Testing). - Sample solution: Dissolve the sample in 3N hydrochloric acid solution, add excess acid. - Test according to the instructions in Food Chemical Codex 6. - Sample: 2 g. - Analysis: Heat at 800°C ± 25°C until constant weight.
4.4. Acidity.
Weigh 2 g of the sample, disperse in 20 ml distilled water. Boil for 1 minute, filter the filtrate. Add 0.1 ml
of phenolphthalein solution (TS) to the filtrate, the filtrate should not show red color. - Test according to Food Chemical Codex 6 (Special Discussion on Cadmium Limit Testing). - Sample solution: Accurately weigh 5 g of the sample, place it in a 50 ml volumetric flask, dissolve the sample in a minimum amount of hydrochloric acid (2:3). Dilute to volume with distilled water, shake well. - Test according to Food Chemical Codex 6 (Special Discussion on Pyrolidindithio Carbamat APDC). - Sample: 2 g - Sample: 2 g - Analysis: Place the sample in a 200 ml flask, dissolve the sample in 20 ml acetic acid (1:4) solution. Dilute to about 150 ml with distilled water, shake well. Precipitate all zinc using a thiourea solution (TS), dilute to volume with distilled water. Filter through dry filter paper, discard the filtrate from the initial stage, then take 100 ml of the filtrate obtained. Add a few drops of sulfuric acid solution to the filtrate. Evaporate to dryness on a water bath and in a pre-weighed dish. After the ammonium salt has completely evaporated, heat the dish at 800°C ± 25°C until constant weight and weigh. The residue weight should not exceed 5 mg.
5.3. Quantitative Analysis - Sample: Weigh 1.5 g of freshly calcined preparation. - Analysis: Dissolve the sample and 2.5 g of ammonium chloride in
50 ml of 1N sulfuric acid, gently heat if necessary. When the sample is completely dissolved, add a few drops of methyl orange solution (TS) and titrate the excess sulfuric acid with sodium hydroxide solution.
Not to exceed 3.0 mg/kg.
Not to exceed 10.0 mg/kg.
Not to exceed 0.5%.
4.3. Quantitative Determination of Zinc Oxide Content in the Product After Calcination
shall not be less than 99.0%.
5.3. Quantitative analysis - Test according to Food Chemical Codex 6 (specific chapter on selenium limit test, Method I - Appendix III B). - Sample: 200 mg. - Sample: Weigh 175 mg of the monohydrate form or 300 mg of the heptahydrate form. - Analysis: Dissolve the sample in 100 ml distilled water, add 5 ml of ammonia-ammonium chloride buffer solution (TS) and add 0.1 ml of eriochrome black T solution (TS). Titrate with sodium EDTA 0.05M solution until the solution turns a clear blue color.
Each milliliter of sodium EDTA 0.05M solution is equivalent to 8.973 mg ZnSO4.H2O or 14.38 mg ZnSO4.7H2O.
Zinc oxide preparation is in white, fine amorphous powder form. When exposed to air, it may gradually absorb
6. Packaging and storage Keep in sealed packaging without air.
Insoluble in water, insoluble in alcohol; soluble in
dilute acids and strong alkalis.
When heated, the sample turns yellow, and this yellow
K
Monohydrate form: 7445-19-7.
color will disappear upon cooling the sample.
Not more than 1.0%.
Test according to the guidance at Food Chemical Codex 6
(Qualitative Study of Zinc). - Sample solution: Dissolve the sample in 3N hydrochloric acid solution, with excess acid.
Test according to the guidance at Food Chemical Codex 6. - Sample: 2 g. - Analysis: calcine at 800°C ± 25°C until constant weight.
Weigh 2 g of the sample, disperse it in 20 ml of distilled water. Boil for 1 minute, filter the filtrate. Add 0.1 ml of phenolphthalein solution (TS) to the filtrate, which must not turn red.
- Test according to Food Chemical Codex 6 (limit test for cadmium). - Sample solution: Accurately weigh 5 g of the sample, place it in a 50 ml volumetric flask, dissolve the sample in a minimum amount of hydrochloric acid (2:3) solution. Dilute to volume with distilled water, shake well.
- Test according to Food Chemical Codex 6 (pyrolidindithio carbamat APDC study). - Sample: 2 g - Sample: 2 g - Analysis: Place the sample in a 200 ml flask, dissolve the sample in 20 ml of acetic acid (1:4) solution. Dilute to approximately 150 ml with distilled water, shake well. Precipitate all zinc using thioacetamide solution (TS), dilute to volume with distilled water. Filter through dry filter paper, discard the initial filtrate, then take 100 ml of the filtrate. Add a few drops of sulfuric acid solution to the obtained filtrate. Evaporate to dryness on a hot plate and in a previously weighed dish. Calcine the dish until the ammonium salt is completely volatilized, then calcine at 800°C ± 25°C until constant weight and weigh. The residue weight shall not exceed 5 mg.
5.3. Quantitative Determination - Sample: Weigh 1.5 g of freshly calcined product. - Analysis: Dissolve the sample and 2.5 g of ammonium chloride in 50 ml of 1N sulfuric acid, heat gently if necessary. When the sample is completely dissolved, add a few drops of methyl orange solution (TS) and titrate the excess sulfuric acid with sodium hydroxide solution.
xuất hiện màu đỏ. - Thử theo Food chemical codex 6 (chuyên luận Thử 
giới hạn cadmi). - Dung dịch mẫu thử: Cân chính xác 5 g mẫu thử, cho 
vào bình định mức 50 ml, hòa tan mẫu thử trong một 
lượng tối thiểu dung dịch acid hydrocloric (2:3). Pha 
loãng đến đủ thể tích bằng nước cất, lắc đều. - Thử theo Food chemical codex 6 (chuyên luận Thử 
Test according to Food Chemical Codex 6 (specific chapter on zinc qualitative test). - Sample solution: Dissolve the sample in 3N hydrochloric acid solution, add a little excess acid. - Test according to Food Chemical Codex 6. - Sample: 2 g. - Analysis: Calcine at 800°C ± 25°C until constant weight.
pyrolidindithio carbamat APDC). - Mẫu thử: 2 g - Mẫu thử: 2 g - Phân tích: Cho mẫu thử vào bình 200 ml, hòa tan mẫu 
thử trong 20 ml dung dịch acid acetic (1:4). Pha loãng 
đến khoảng 150 ml bằng nước cất, lắc đều. Kết tủa 
hoàn toàn kẽm bằng dung dịch amoni sulfid (TS), pha 
loãng đến thể tích bằng nước cất. Lọc qua giấy lọc khô, 
loại bỏ dịch lọc của giai đoạn đầu, tiếp theo lấy 100 ml 
dịch lọc. Thêm vào dịch lọc thu được vài giọt dung dịch 
acid sulfuric. Cho bay hơi đến khô trên bể cách thủy và 
trong một đĩa đã cân bì. Nung chén cho đến khi muối 
amoni bay hơi hết, sau đó nung tại 800oC ± 25oC, đến 
khối lượng không đổi và cân. Khối lượng cặn không 
được quá 5 mg.  
5.3. Định lượng - Mẫu thử: Cân 1,5g chế phẩm mới nung. - Phân tích: Hòa tan mẫu thử và 2,5g amoni clorid trong 
50 ml acid sulfuric 1N, đun nhẹ nếu cần. Khi mẫu thử 
tan hoàn toàn, thêm vài giọt dung dịch da cam methyl 
(TS) và chuẩn độ acid sulfuric dư bằng dung dịch natri 
hydroxide 1 N. Each milliliter of 1N sulfuric acid is equivalent to
40.69 mg of ZnO.
6. Packaging and storage Keep in sealed packaging.