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GB 14757-2010 English PDF

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GB 14757-2010: National food safety standards -- Food additives -- Niacin
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GB 14757: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
GB 14757-2010English279 Add to Cart 3 days [Need to translate] National food safety standards -- Food additives -- Niacin Valid GB 14757-2010
GB 14757-1993English239 Add to Cart 2 days [Need to translate] Food additive. Nicotinic acid Obsolete GB 14757-1993

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Basic data

Standard ID GB 14757-2010 (GB14757-2010)
Description (Translated English) National food safety standards -- Food additives -- Niacin
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 12,194
Date of Issue 2010-12-21
Date of Implementation 2011-02-21
Older Standard (superseded by this standard) GB 14757-1993
Regulation (derived from) Ministry of Health Bulletin No. 19 of 2010
Issuing agency(ies) Ministry of Health of the People's Republic of China
Summary This Chinese standard applies to chemical synthesis of food additives niacin.

GB 14757-2010: National food safety standards -- Food additives -- Niacin

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
National food safety standards - food additives - Niacin National Standards of People's Republic of China National Food Safety Standard Food Additives niacin Issued on. 2010-12-21 2011-02-21 implementation People's Republic of China Ministry of Health issued

Foreword

This standard replaces GB 14757-1993 "Food Additives niacin" This standard compared with GB 14757-1993 main changes are as follows. - Loss on drying index from 1% revised to 0.5%; - Added Infrared Spectroscopy; - Increased arsenic indicators. The Standard Annexes A and B are normative appendix. This standard replaces the standards previously issued as follows. --GB 14757-1993. National Food Safety Standard Food Additives niacin

1 Scope

This standard applies to chemical synthesis of food additives niacin.

2 Normative references

The standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard. 3 chemical name, molecular formula, molecular mass and structural formula 3.1 Chemical Name Pyridine-3-carboxylic acid Formula 3.2 C6H5NO2 3.3 formula COOH 3.4 relative molecular mass 123.11 (according to 2007 international relative atomic weight) 4. Technical Requirements 4.1 Sensory requirements. comply with the requirements of Table 1. Table 1 Sensory requirements Project requires test methods White or white color proper amount of sample is placed in 50mL beaker, observe the color in natural light And texture. Smell it. Odour odorless or has a slight odor Organizational status crystalline powder 4.2 Physical indicators. in accordance with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Niacin (dry basis), w /% 99.5 ~ 101.0 Appendix A A.4 Loss on drying, w /% ≤ 0.5 A.5 in Appendix A Table 2 (Continued) physical and chemical indicators Chloride (Cl dollars), w /% ≤ 0.02 A.6 in Appendix A Residue on ignition, w /% ≤ 0.1 Appendix A A.7 Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.8 Melting point/℃ 234 ~ 238 Appendix A, A.9 Heavy metals (Pb)/(mg/kg) ≤ 20 Appendix A A.10

Appendix A

(Normative) Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, according to the relevant provisions of the operation, the operation need to be careful! If splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid, to be carried out in a fume hood. A.2 General Provisions The reagents used in this standard, unless otherwise noted, only in the analysis confirmed analytically pure reagents and GB/T 6682-2008 in Regulation Given three water. Standard Solution, Test Method for preparation and products required, did not indicate when the other requirements, according to GB/T 601, GB/T 603 Provisions prepared. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 95% ethanol. A.3.1.2 2,4- dinitro chlorobenzene. A.3.1.3 Potassium hydroxide solution. take 3.5 g of potassium hydroxide, add 100 mL ethanol to dissolve, after resting the supernatant. A.3.1.4 sodium hydroxide solution. 4 g/L. A.3.1.5 copper sulfate solution. 125 g/L. A.3.2 Identification method A.3.2.1 Identification of the pyridine ring A.3.2.1.1 Method summary Niacin plus 2,4-dinitro-chlorobenzene melted to form a quaternary ammonium compound, and then potassium hydroxide solution, which was purple (Vongerichten reaction). A.3.2.1.2 analysis step Laboratory samples taken from about 4 mg, 8 mg 2,4- plus dinitro chlorobenzene, Research uniform, a test tube, slowly heated to melt, and then the number of heating Seconds, cooled to room temperature, 3 mL ethanol solution of potassium hydroxide. That was purple. A.3.2.2 Identification precipitation reaction with copper sulfate A.3.2.2.1 Method summary Carboxyl group-containing nicotinic acid, neutralized with sodium hydroxide, the case of copper sulfate to generate light blue nicotinic acid precipitation. A.3.2.2.2 analysis step Take about 50 mg laboratory samples, add 20 mL of water dissolved a solution of sodium hydroxide solution to neutral reaction in case of litmus paper, add 3 mL Copper sulfate solution, that is slowly precipitated pale blue precipitate. A.3.2.3 UV spectrophotometry A.3.2.3.1 Method summary Nicotinic acid and nicotinamide aqueous solution by spectrophotometry, absorption maximum at 262 nm wavelength are, nicotinic acid in 237 nm Wavelength of minimum absorption; nicotinamide at 245 nm wavelength of minimum absorption, the absorption of niacin ratio A237nm/A262nm 0.35 to 0.39; Nicotinamide absorbance ratio A245nm/A262nm 0.63 to 0.67. Therefore, this method can be used to distinguish between niacin and niacinamide. A.3.2.3.2 analysis step Take laboratory sample amount, add water produced per 1 mL of 20 μg of the solution, according to spectrophotometric method (Chinese Pharmacopoeia 2005 edition of two Appendix Ⅳ A) Determination of maximum absorption at a wavelength of 262 nm ± 1 nm, the minimum absorption at 237 nm ± 1 nm in wavelength; 237 nm ± 1 nm absorbance wavelength and absorbance ratio of 262 nm ± 1 nm wavelength should be 0.35 to 0.39. A.3.2.4 infrared absorption spectroscopy Using potassium bromide tablet method according to GB/T 6040 test, the laboratory sample infrared light absorption spectrum with a control of the map Induced (control profile see Appendix B). A.4 Determination of niacin A.4.1 Method summary Phenolphthalein as an indicator, titration with aqueous sodium hydroxide standard solution titration sample, according to standard titration of sodium hydroxide solution consumed The amount was calculated content of C6H5NO2 meter niacin. The results and titration with blank test correction. A.4.2 Reagents and materials A.4.2.1 sodium hydroxide standard titration solution. c (NaOH) = 0.1 mol/L. A.4.2.2 phenolphthalein indicator solution. 10 g/L ethanol solution. A.4.3 Analysis step Weigh about 0.3 g laboratory samples, accurate to 0.000 1 g, add 50 mL freshly boiled and cooled water dissolved, add 3 drops of phenol Phthalate indicator solution, titration with sodium hydroxide standard solution titration to pink. A.4.4 Calculation Results Niacin (in C6H5NO2 meter) mass fraction 1w, expressed in%, according to formula (A.1) Calculated. () 100 (1) 1000 VV c Mw mw - × × = ×× - ×% (A.1) Where. V - consumption of sodium hydroxide standard titration solution volume value in milliliters (mL); 0V - Numerical volume consumed sodium hydroxide standard titration blank test solution, in milliliters (mL); c - sodium hydroxide standard titration solution actual concentration values, units of moles per liter (mol/L); m - the quality of the laboratory sample value in units of grams (g); 2w --A.5 measured value loss on drying,%; M - molar mass values of nicotinic acid in grams per mole (g/mol) [M (C6H5NO2) = 123.1]. The absolute difference between two parallel determination of not more than 0.3%. A.5 Determination of loss on drying A.5.1 Analysis step Weigh about 1.0 g laboratory samples, accurate to 0.000 1 g, has been placed at 105 ℃ ± 2 ℃ drying to constant weight flat weighing bottle, At 105 ℃ ± 2 ℃ drying 1h, into the cooled to room temperature in a desiccator and weighed. A.5.2 Calculation Results Niacin drying loss mass fraction 2w and its value is expressed in%, according to formula (A.2) Calculated. m mw - = ×% (A.2) Where. 1m - the total mass of the laboratory sample values before drying and weighing bottles in grams (g); 2m - After drying the total mass of the sample and weighing bottle laboratory values, expressed in grams (g); m - mass values laboratory sample in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.05%. A.6 Determination of chloride A.6.1 Reagents and materials A.6.1.1 nitric acid solution. 105 → 1000. A.6.1.2 silver nitrate test solution. 0.1 mol/L. A.6.1.3 Preparation of standard solution of sodium chloride Weigh about 0.165 g sodium chloride, to the nearest 0.000 2 g, set 1000 mL volumetric flask, add water to dissolve and dilute to the mark, Shake, as the stock solution. Before use, the precise amount of stock solution of 10 mL, 100 mL flask, diluted with water to the mark, shake, that was (mL per one equivalent To 10μg of Cl-). A.6.2 Analysis step Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix Ⅷ A portion of two chloride test method, as follows. Weigh 0.25 g ± 0.01g laboratory samples. Dissolved in water to make 25 mL, 10 mL plus nitric acid solution, placed in 50 mL colorimetric Tube, add water to make 40 mL, shake, that was the test solution; at the same time take 5.0 mL of sodium chloride solution was placed in a standard other than 50 mL Color tube, plus 10 mL of nitric acid solution, add water to make 40 mL, shake, that was a control solution. In the test solution and control solution Were added to 1.0 mL of silver nitrate solution, diluted with water to 50 mL, shake, in the dark place 5min, on a black background with the home, the test Fluid and control fluid compared to the turbidity of the test solution is not greater than the control solution turbidity. A.7 Determination of residue on ignition A.7.1 Method summary Sample by adding sulfuric acid sulphate after ignition of the left, with the weight method. A.7.2 Analysis step It weighs about 1.0 g laboratory samples, accurate to 0.000 1 g, placed in a burned to constant weight porcelain crucible at 550 ℃ ± 50 ℃, with Small fire slowly heated to completely carbonized, cooled to room temperature, add 0.5 mL sulfuric moist, low temperature sulfuric acid heated to steam divisible, transfer Into a high-temperature furnace to burn at 550 ℃ ± 50 ℃ constant weight. A.7.3 Calculation Results Residue on ignition niacin mass fraction 3w and its value is expressed in%, according to formula (A.3) Calculated. m mw - = ×% (A.3) Where. 3m - the total mass of the crucible and residue values in grams (g); 4m - crucible mass value in grams (G); m - mass values laboratory sample in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.02%. A.8 Determination of Arsenic A.8.1 Method summary In strongly acidic solution, the sample can be reduced to metallic zinc arsenic into arsine arsine regenerate brown and mercuric bromide paper role Yellow compound. Samples with arsenic standard solution using the same method of treating the resulting brown compound compared to the sample in order to check the arsenic salt limit. A.8.2 Analysis step Weigh 5.0 g ± 0.01 g laboratory samples weighed 10 mL ± 0.05 mL limit of arsenic standard solution (per 1 mL solution corresponds to 1 μg Arsenic), respectively GB/T 5009.76-2003 Method 5.2.2 first dry ashing sample after treatment, according to the second law Gutzeit assay samples. Specimen Gutzeit No deeper than the standard Gutzeit. Determination of the melting point A.9 Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix Ⅵ C section two first melting point determination method, as follows. Take the test amount, in flat weighing bottle after 105 ℃ ± 2 ℃ drying 1h, cooling into a desiccator to room temperature, amount, Set capillary melting point measurement (referred to capillary hard glass is made from neutral, more than 9 cm long, inner diameter of 0.9 ~ 1.1 mm, wall Thickness of 0.10 mm ~ 0.15 mm, one end of the fusion seal; when the thermometer is immersed in transmission fluid temperature at 6 cm above the tube length should be increased, so that Exposed surface 3 cm above), tap the wall or by means of a suitable length of a clean glass tube, placed vertically on the surface of the dish or other suitable hard Qualitative objects from the capillary into the catchy its free fall, repeated several times, the powder tightly assembled capillary melting terminated. Dress The height of the test is 3 mm. Another thermometer (sub-dip type, with 0.5 ℃ scale, the melting point was determined by reference correction) into Costumes transmission fluid temperature (silicone oil or liquid paraffin) container so that the bottom portion of the bottom of the thermometer mercury ball away from the container more than 2.5 cm (with Surface distance of 2.5 cm or more) on a heated vessel, a thermometer mercury ball and heater; adding transmission fluid temperature to allow liquid transmission fluid temperature after heating Suitable dip in the sub-line of the thermometer. When the transmission fluid temperature heating, as soon as the temperature rises to a predetermined relatively low melting point lower limit of about 10 ℃, will be equipped with the test Products capillaries immersed in transmission fluid temperature, attached to the thermometer (available rubber band or a capillary tube clamp), it shall be so content capillary Suitable mercury thermometer was in the middle of the ball; heating was continued to adjust the heating rate per minute rising 1.0 ℃ ~ 1.5 ℃, the heating must be constantly stirring So that transmission fluid temperature to maintain a uniform temperature recorded for the sample temperature to melt in the early melting of the whole repeated measured three times and averaged. A.10 Determination of Heavy Metals A.10.1 reagents and materials A.10.1.1 nitrate. A.10.1.2 sulfuric acid. A.10.1.3 hydrochloric acid. A.10.1.4 glycerol. A.10.1.5 ammonium acetate. A.10.1.6 lead nitrate. A.10.1.7 thioacetamide. A.10.1.8 ammonia solution. 400 → 1000. A.10.1.9 sodium hydroxide solution. c (NaOH) = 1 mol/L. A.10.1.10 hydrochloric acid solution. c (HCl) = 2 mol/L. A.10.1.11 hydrochloric acid solution. c (HCl) = 7 mol/L. A.10.1.12 ammonia solution. c (NH3 · H2O) = 5 mol/L. A.10.1.13 phenolphthalein indicator solution. 10g/L ethanol solution. A.10.1.14 acetate buffer (pH3.5). Weigh about 25 g of ammonium acetate, 25 mL water was added after dissolved, and 7 mol L hydrochloric acid/38 mL, Accurately adjusted with 2 mol/L hydrochloric acid solution or aqueous ammonia solution to pH 3.5 (indicating potential method), diluted with water to 100 mL, that is, too. A.10.1.15 thioacetamide test solution. Weigh about 4.0g thioacetamide, to the nearest 0.01 g, add water to dissolve into a 100 mL, home ice Box for storage. Immediately prior to taking 5.0 mL mixture of [the 1 mol/L 15 mL of sodium hydroxide solution, 5.0 mL of water and 20 mL glycerol], plus Above 1.0 mL of thioacetamide solution was heated on a water bath 20s, cooling, use immediately. A.10.1.16 lead standard solution. Weigh about 0.160 g of lead nitrate, accurate to 0.0002g, placed in 1000 mL volumetric flask, add 5 mL Glass After acid and 50 mL of water to dissolve, dilute to the mark, shake, as the stock solution. Before use, pipette 10 mL ± 0.02 mL stock solution, Placed 100 mL volumetric flask, diluted with water to the mark, shake, that was (per 1mL equivalent to 10 μg of Pb). And storage configuration used Glassware shall lead. A.10.2 Analysis steps Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix Ⅷ H Method II test for heavy metals, as follows. Take the residue left under item A.7, add 0.5 mL of nitric acid, evaporated and the vapor is divisible to nitric oxide (or after taking 1.0 g laboratory samples Slowly burn to completely carbonized, cooled to room temperature, 0.5 mL ~ 1.0 mL of sulfuric acid, so just moist, low temperature sulfuric acid heated to divisible, Add 0.5 mL of nitric acid, evaporated to steam after the nitrogen oxide divisible, cooled to room temperature, burning until completely ashed at 500 ℃ ~ 600 ℃), cold To room temperature, add 2 mL of hydrochloric acid, add 15 mL water was evaporated to dryness on a water bath, dropping ammonia solution to phenolphthalein instructions VIS neutral, plus 2 mL acetate buffer (pH3.5), after heat gently to dissolve, displacing A Nessler colorimetric tube, diluted with water to 25 mL; Another test preparation Reagent chamber of the sample solution, evaporated to dryness rear porcelain dish, add 2 mL acetate buffer (pH 3.5) and after 15 mL of water, heat gently to dissolve, Displacement Nessler colorimetric tube B, add lead standard solution 2 mL ± 0.01 mL, then diluted with water to 25 mL; and then were added to the two B Thioacetamide test solution each 2 mL, shake, place 2min, on the same set of paper, from the top down perspective, A color display tube and pipe B , Not deeper.

Appendix B

(Normative) Niacin infrared absorption spectrum Note. Quoted from "Drug IR set," Volume I (1995) Figure B.1 niacin infrared absorption spectrum

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