GB 14758-2010 English PDFUS$329.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 14758-2010: National food safety standards -- Food additives -- Caffeine Status: Valid GB 14758: Historical versions
Basic dataStandard ID: GB 14758-2010 (GB14758-2010)Description (Translated English): National food safety standards -- Food additives -- Caffeine Sector / Industry: National Standard Classification of Chinese Standard: X42 Classification of International Standard: 67.220.20 Word Count Estimation: 14,17 Date of Issue: 2010-12-21 Date of Implementation: 2011-02-21 Older Standard (superseded by this standard): GB 14758-1993 Regulation (derived from): Ministry of Health Bulletin No. 19 of 2010 Issuing agency(ies): Ministry of Health of the People's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 acid or cyanuric acid as raw materials in chemical synthesis and tea as raw material extraction method were food additive caffeine. GB 14758-2010: National food safety standards -- Food additives -- Caffeine---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 - caffeine National Standards of People's Republic of China National Food Safety Standard Food Additives Caffeine Issued on. 2010-12-21 2011-02-21 implementation People's Republic of China Ministry of Health issued ForewordThis standard replaces GB 14758-1993 "food additive caffeine." This standard compared with GB 14758-1993, the main changes are as follows. - Described by the appearance of white crystalline powder to white or very light yellow green crystalline powder; - Caffeine content allowed by the relative difference between the differential absolute difference of 0.3% to 0.2%; - Added Infrared Spectroscopy; - Increase the clarity of the project; - 0.0003% of arsenic from the index changed to 2 mg/kg; - Added chromatographic purity requirements. The Standard Annexes A and B are normative appendix Appendix C is informative appendix. This standard replaces the standards previously issued as follows. - GB 14758-1993 National Food Safety Standard Food Additives Caffeine1 ScopeThis standard applies to acetic acid or cyanide as raw materials chemical synthesis and extraction method of tea as raw materials obtained food additive coffee because.2 Normative referencesThe standard file referenced in the application of this standard is essential. For dated references, only the edition date of the note Apply 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 1,3,7-trimethyl-xanthine Formula 3.2 Or C8H10N4O2 C8H10N4O2 · H2O 3.3 formula 3.4 relative molecular mass Caffeine Anhydrous. 194.19 (according to 2007 international relative atomic mass) A water-caffeine. 212.21 (according to 2007 international relative atomic mass) 4. Technical Requirements 4.1 Sensory requirements. comply with Table 1. Table 1 Sensory requirements Project requires test methods Color white or green belt extremely popular and mercerized take appropriate sample is placed in a clean, dry beaker, under natural light, observe the color and texture, smell the odor. After gargling with warm water and enjoy the taste. Taste, smell bitter, odorless Organization Status needle crystal or crystalline powder or granules. Having weathering 4.2 Physical indicators. to comply with Table 2. CH3 CH3 CH3 Table 2. Physical and chemical indicators Item Index Test Method Caffeine (C8H10N4O2, dry basis), w /% 98.5 ~ 101.0 Appendix A A.4 Loss on drying, w /% ≤ 0.5 (Anhydrous) Appendix A A.5 8.5 (aqueous) Residue on ignition, w /% ≤ 0.1 A.6 in Appendix A No other alkaloids precipitate A.7 in Appendix A Chromatographic purity, w /% Single impurity ≤ 0.1 Appendix A A.8 Total impurities ≤ 0.1 Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.9 Melting point/℃ 235.0 ~ 237.5 Appendix A A.10 Clarity test (20g/L solution) through a test A.11 in Appendix A Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.12 Easy carbide by test A.13 in Appendix AAppendix 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, should be used with caution. If splash 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 stated in the analysis using only recognized as analytical reagents and GB/T 6682-2008 specified in Three water. The test method used in the standard titration solution, impurities measured by standard solution, preparations and products, not specified in other requirements, according GB/T 601, GB/T 602, the provisions of the preparation of GB/T 603's. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 hydrochloric acid. A.3.1.2 potassium chlorate. A.3.1.3 ammonia solution. 10 → 100. A.3.1.4 hydrochloric acid solution. 10 → 100. A.3.1.5 sodium hydroxide solution. 40g/L. A.3.1.6 iodine solution. 0.1 mol/L. A.3.2 Analysis step A.3.2.1 purple urea acid coloring test Laboratory samples taken from about 10.0 mg, add 1mL hydrochloric acid solution and 0.1 g of potassium chlorate, on a water bath evaporated, the residue in case of ammonia that is significant purple, Plus the number of sodium hydroxide solution was dropped, purple disappeared. A.3.2.2 caffeine precipitation reaction with iodine and hydrochloric acid test solution Take 5 mL of saturated aqueous laboratory sample, add 5 drops of iodine solution, no precipitation occurs; plus 3 drops of hydrochloric acid solution, which appears red-brown The precipitate can be dissolved in a slight excess of sodium hydroxide solution. A.3.2.3 Infrared Spectroscopy Using potassium bromide tablet method according to GB/T 6040 test, IR should control profile laboratory sample (see Appendix B) Consistent. A.4 Determination of caffeine A.4.1 Reagents and materials A.4.1.1 acetic anhydride. A.4.1.2 benzene. A.4.1.3 perchloric acid standard titration solution. c (HClO4) = 0.1 mol/L. A.4.2 Instruments and Equipment Titrator. A.4.3 Analysis step Take about 0.4 g laboratory samples, accurate to 0.000 2 g, add 40 mL of acetic anhydride, dissolved by heating, cooling, add 80 mL of benzene, with a high Standard acid droplets given titration, potentiometric method indicates the end, the results and titration with blank test correction. A.4.4 Calculation Results Caffeine (C8H10N4O2 to count) mass fraction w1, expressed in%, according to formula (A.1) Calculated. (11000 VV c Mw mw - × × = ×× - × () )% (A.1) Where. V-- laboratory sample consumption volume of perchloric acid standard solution, in milliliters (mL); V0-- blank test consumption volume perchloric acid standard solution, in milliliters (mL); Molar concentration c-- perchloric acid titration solution, expressed in moles per liter (mol/L); Numerical quality m-- laboratory sample in grams (g); Loss on drying of the value w2--,%; M - molar mass values of caffeine in units of grams per mole (g/mol) [M (C8H10N4O2) = 194.2] Take the arithmetic mean of the parallel determination results of the measurement results, the absolute difference between two parallel determination of not more than 0.2%. A.5 Determination of loss on drying A.5.1 Analysis step Take 1.0 g laboratory samples, accurate to 0.000 2 g, was placed at 80 ℃ dried to constant weight weighing bottle, precisely weighed, placed in 80 ℃ Oven dried to constant weight. A.5.2 Calculation Results Loss on drying sample mass fraction to 2w and its value is expressed in%, according to formula (A.2) Calculated. 100m mw mm - = × -% (A.2) Where. Numerical m1-- laboratory samples before drying and weighing bottles total mass in grams (g); After drying m2-- numerical laboratory samples weighing bottle and the total mass in grams (g); Numerical m3-- weighing bottle mass 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 residue on ignition A.6.1 Reagents and materials sulfuric acid. A.6.2 Analysis step Take 1.0 g laboratory samples, accurate to 0.001 g, are placed till constant weight at 750 ℃ ± 50 ℃ porcelain crucible, low heat and slowly add Heat to completely carbonized. After cooling to room temperature, 0.5 mL ~ 1 mL of sulfuric acid so moist, cold sulfuric acid heated to steam divisible, moved into high temperature Furnace, burning at 750 ℃ ± 50 ℃ high temperature furnace to constant weight. A.6.3 Calculation Results The mass fraction of residue on ignition in 3w and its value is expressed in%, according to formula (A.3) Calculated. m mw - = ×% (A.3) Where. Numerical m4-- crucible and residue total mass, in grams (g); Numerical m5-- crucible mass in grams (g); m-- mass of the sample value in units of 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%. Determination A.7 other alkaloids A.7.1 Reagents and materials Potassium mercuric iodide test solution. Take 1.36g mercury dichloride, add water to dissolve 60mL, the other to take potassium iodide 5g, add water to dissolve 10mL, the two Liquid mixing, dilution after mixing with water to 100mL. A.7.2 Analysis step Weigh 1 g laboratory sample, add 50 mL of water, 10 mL of the solution add 3 drops of potassium mercuric iodide test solution shall not cause precipitation. A.8 Determination of chromatographic purity A.8.1 Reagents and materials A.8.1.1 anhydrous sodium acetate. A.8.1.2 acetonitrile. chromatography. A.8.1.3 tetrahydrofuran. chromatography. A.8.1.4 glacial acetic acid. A.8.1.5 theophylline reference. A.8.1.6 caffeine reference. A.8.2 Instruments and Equipment High performance liquid chromatography. A.8.3 Chromatography conditions Recommended chromatographic columns and typical operating conditions are shown in Table A.1, caffeine HPLC system suitability test diagram see Figure C.1, Relative retention time of the components in Table C.1. Others can achieve the same degree of separation columns and chromatographic conditions can be used. φ Table A.1 column chromatography and typical operating conditions Column octadecyl silane bonded silica gel column (particle size 5 μm, φ4.6 mm × 150 mm stainless steel column) The mobile phase Weigh about 1.64 g of anhydrous sodium acetate, accurately weighed, dissolved in water and diluted to 2000 mL, and mix. Take 1910 mL, add acetonitrile 50 mL, THF 40 mL, mixed with glacial acetic acid adjusted pH = 4.5, Mixing, filtering, degassing Flow rate of about 1 mL/min Detector wavelength 275 nm A.8.4 Analysis step A.8.4.1 reference solution. Weigh about 2 mg theophylline reference, accurate to 0.000 1 g, set 100 mL volumetric flask, add about 50 mL stream The mobile phase was shaken, and dissolved with ultrasound, mobile phase and dilute to volume, and mix. A.8.4.2 Preparation of system suitability test solution. Weigh about 5.0 mg caffeine reference, accurate to 0.000 1 g, set 25 mL volumetric flask, Add 5.0 mL reference solution and 10 mL of mobile phase, shaking, sonication, then the mobile phase and dilute to volume, and mix. A.8.4.3 laboratory sample preparation solution. Weigh about 10 mg of caffeine laboratory samples, accurate to 0.000 1 g, set 50 mL volumetric flask, Add 10 mL of mobile phase, shaking, sonication, then the mobile phase and dilute to volume, and mix. A.8.4.4 Instrument Preparation. According to high performance liquid chromatography procedures to prepare the instrument, set a flow rate of 1 mL/min, the detection wavelength was 275 nm, With the mobile phase equilibrium apparatus, the start of the injection operation. A.8.4.5 System suitability test. Take 10 μL injection system suitability test solution, record the chromatograms, theophylline and caffeine relative retention times Turn around 0.69,1.0; degree of separation between the two peaks is not less than 6.0; each peak tailing factor T≤2.0. A.8.4.6 Determination. Take the mobile phase and sample solution 10 μL injections twice to record caffeine chromatogram peak retention time. By area Calculate the impurity content normalization method. A.8.5 result of the calculation (area normalization method) The mass fraction of impurities in 4w and its value is expressed in%, according to formula (A.4) Calculated. 4 × 100 = Σ hetero% (A.4) Where. A hetero - impurity peak area (in addition to the solvent peak and the peak outside); ΣA-- area of all peaks and (excluding the solvent peak). A.9 Determination of Arsenic Take 1.0 g ± 0.01 g laboratory samples, add 20 mL of water, dissolved by heating, cooled to room temperature, transfer of 100 mL Erlenmeyer flask, 5 mL of Hydrochloric acid, 5 mL potassium iodide solution, 5 drops of acidic stannous chloride solution, in accordance with the provisions of GB/T 5009.76-2003 Gutzeit method performed. Determination of the melting point A.10 Press the "People's Republic of China Pharmacopoeia" 2005 edition two Appendix VI C melting point of the first assay method. Here's how. Take laboratory sample amount, reduced to powder, dried in an oven at 80 ℃ for 4 h, dispensing amount, set by capillary melting point measurement (Jane Said capillary tube, made of neutral glass hard, more than 9 cm long, inner diameter of 0.9 mm ~ 1.1 mm, wall thickness of 0.10 mm ~ 0.15 mm, End fusion seal; when the thermometer is immersed in transmission fluid temperature at 6 cm above the tube length should be increased, so that the exposed surface 3 cm or more), the light Hit the wall or by means of a suitable length of a clean glass tube is placed vertically on the surface of the dish or other suitable rigid object from the capillary into the catchy The free fall, repeated several times, the powder tightly assembled capillary melting terminated. Laboratory sample loading height of 3 mm. The other will be warm Meter (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) tolerance Vessel, so that the bottom portion of the bottom of the thermometer mercury ball away from the container more than 2.5 cm (with a heated vessel, heater and thermometer mercury ball 2.5 cm above the upper surface distance); adding transmission fluid temperature so that the heat transmission fluid temperature level after the appropriate line of the sub-immersion thermometer. The transmission fluid temperature heating, When the temperature rises to a predetermined relatively low melting point lower limit at about 10 ℃, the lab will be equipped with a capillary sample immersed in transmission fluid temperature, a thermometer attached On (available rubber band or capillary fixed), it shall be so suitable capillary contents of mercury in the thermometer ball middle; heating was continued, warming to adjust Rate increased 1.0 ℃ ~ 1.5 ℃ per minute, stirring constantly so that when heated to be transmission fluid temperature to maintain a uniform temperature recorded at the beginning of the laboratory sample melt Temperature to melt the whole time, repeated measured three times and averaged. A.11 Determination of Clarity A.11.1 reagents and materials A.11.1.1 methenamine solution. 10 g/L. Preparation A.11.1.2 turbidity standard stock solution. Weigh dried at 105 ℃ to constant weight of 1.00 g hydrazine sulfate, 100 mL flask, add water Amount to dissolve, if necessary, can be warmed in a water bath 40 ℃ dissolved, and diluted with water to the mark, shake, place 4 h ~ 6 h; of this solution Methenamine solution with an equal volume (100g/L) mixing, shake, standing in the dark at 25 ℃ 24h, that is, too. The liquid home cold place away from light, Available within two months use, shake well before use. Preparation A.11.1.3 turbidity standard stock solution. Take 15.0 mL stock solution turbidity standard, set in 1 000 mL volumetric flask, diluted with water to the mark, Shake, check amount, set 1cm absorption cell, according to the UV - visible spectrophotometry ( "People's Republic of China Pharmacopoeia" 2005 edition of Appendix IV A), At a wavelength of 550 nm is measured, the absorbance should be within the range of 0.12 to 0.15. The solution should be within 48h use Shake well before use. No. A.11.1.4 0.5 turbidity standard solution preparation. Take turbidity standard 2.50 mL stock solution to 100 mL volumetric flask, add 97.50 mL of water to the mark, Shake, that was. This solution should be prepared just before use, shake well before use. A.11.2 Analysis steps Press the "People's Republic of China Pharmacopoeia" 2005 edition two Appendix B Ⅸ clarity test method. Weigh (1.0 ± 0.01) g laboratory sample Product, add 50 mL of water, heated to boiling, cooled to room temperature, compared with the same volume of water or a 0.5 turbidity standard solution No. 6. If the turbidity can not be more than No. 0.5 turbidity standard solution deeper. A.12 Determination of Heavy Metals A.12.1 reagents and materials A.12.1.1 nitrate. A.12.1.2 glycerol. A.12.1.3 ammonium acetate. A.12.1.4 lead nitrate. A.12.1.5 thioacetamide. A.12.1.6 hydrochloric acid solution. c (HCl) = 2 mol/L. A.12.1.7 ammonia solution. c (NH3 · H2O) = 5 mol/L. A.12.1.8 sodium hydroxide solution. c (NaOH) = 1 mol/L. A.12.1.9 hydrochloric acid solution. c (HCl) = 7 mol/L. A.12.1.10 acetate buffer (pH3.5). Weigh about 25 g of ammonium acetate, accurate to 0.01 g, add 25 mL of water dissolved, add 7 mol / L hydrochloric acid solution, 38 mL, 2 mol L hydrochloric acid solution with/or a 5 mol/L aqueous ammonia solution, the pH adjusted to accurately 3.5 of 5 (pH meter), diluted with water to 100 mL. A.12.1.11 thioacetamide test solution. Weigh about 4 g thioacetamide, to the nearest 0.01 g, add water to dissolve into a 100 mL, set the refrigerator Saved. Immediately prior to taking 5.0 mL mixture (by a 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.12.1.12 lead standard solution. Weigh about 0.160 g of lead nitrate, accurate to 0.0002g, placed in 1000 mL volumetric flask, add 5 mL of nitric acid After dissolution with 50 mL of water, dilute to the mark, shake, as the stock solution. Before use, Pipette (10 ± 0.02) mL stock solution, put 100 mL volumetric flask, diluted with water to the mark, shake, that was (per 1mL equivalent to 10 μg of Pb). Preparation and storage with glass instrument Device shall not contain lead. A.12.2 Analysis steps Press the "People's Republic of China Pharmacopoeia" 2005 edition Appendix Ⅷ H method first heavy metal inspection method. Here's how. Take 25 mL Nessler colorimetric tube two, A tube was added 0.5 mL ± 0.005 mL (lead 5.0 μg) of lead (Pb) and 2 mL standard solution B After formate buffer, diluted with water to 25 mL, 0.5 g Weigh other laboratory samples, accurate to 0.01 g, placed Nessler colorimetric tube acetate tube, Add 20 mL of water, heated to dissolve, cooled to room temperature, add 2 mL acetate buffer (pH3.5) and the amount of water into a 25 mL (filter if necessary Guo), if the solution is colored, can be a small amount of a dilute solution of caramel solution or other non-interfering A colored solution in the tube, so that it is consistent with the pipe B; And then were added to the two B thioacetamide test solution in each of 2 mL, shake, place 2min, on the same set of paper, from the top down perspective, acetic Tube A comparison with the color tube showing no deeper. Determination A.13 easy to charcoals A.13.1 reagents and materials A.13.1.1 sulfuric acid solution. 94.5% - 95.5% (mass fraction). A.13.1.2 cobalt chloride solution. take cobalt chloride (CoCl2.6H2O), dissolved in hydrochloric acid solution (1 → 40), making a 1 000 mL, 5.00 to take the liquid mL of, set iodometric 250 mL flask, add 5 mL of hydrogen peroxide solution of sodium hydroxide followed by 15 mL of test solution (200g/L), boiled for 10 min cooled, Added 2 g of potassium iodide and 20 mL of sulfuric acid solution (1 → 4), until the precipitate was dissolved......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 14758-2010_English be delivered?Answer: Upon your order, we will start to translate GB 14758-2010_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 14758-2010_English with my colleagues?Answer: Yes. 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