Some standard content:
National Standard of the People's Republic of China
Food additive
β-carotene
Food additiveβ-carotene
UDC547.979664
GB8821-88
This standard applies to β-carotene obtained by chemical synthesis with vitamin A acetate as the starting material, as a food coloring and nutritional enhancer.
Molecular formula: CH
Molecular weight: 536.88 (according to the 1983 International Atomic Weight Table). Structural formula:
Technical requirements
1.1 Appearance: This product is purple or red crystalline powder. Odorless and tasteless, the product appearance becomes lighter after being affected by light, heat and air. This product is soluble in carbon disulfide, benzene, trinitromethane, slightly soluble in ether, petroleum ether, food oil, cyclohexane, and almost insoluble in ethanol, water, acid and alkali. 1.2 Items and indicators
Absorbance ratio
(1)AssX10/Aso
(2)Ass/As
Content (in CH4), %
Arsenic salt (in As), %
Heavy metal (in Pb), %
Melting point, ℃ (decomposition point)
Residue on ignition, %
Dissolution test (1g/100mL)
2 Test method
1.14~1.18
96.0~101.0
≤0.0003
176~182
Unless otherwise specified, the reagents used in the test are analytical pure reagents, water is distilled water or water of equivalent purity, solution is aqueous solution, and the instruments and equipment are general laboratory equipment.
2.1 Identification
Approved by the State Food and Drug Administration in 1988-0222
Implemented on 1988-08-01
GB 8821-88
Principle: β-carotene is a conjugated double bond compound with three absorption peaks in the ultraviolet spectrum (455nm, 483nm, 340nm). The ratio of A4/A and Aas/As is used to control the cis isomers and carotenoids in β-carotene. 2.1.1 Reagents and solutions
2.1.1.1 Cyclohexane.
2.1.1.2 Chloroform (GB682--78). 2.1.1.3 Preparation of sample solution
Solution A: Take 0.05g of this product and weigh it accurately, place it in a 100mL brown volumetric flask, add 10mL of chloroform, dissolve it first, immediately dilute it to the mark with cyclohexane, and shake it well. Take 5.0mL of this solution, place it in a 100mL brown volumetric flask, dilute it to the mark with cyclohexane, and shake it well.
Solution B: Take 5.0mL of solution A, place it in a 50mL brown volumetric flask, dilute it to the mark with cyclohexane, and shake it well. 2.1.2 Instruments and equipment
2.1.2.1 UV spectrophotometer.
2.1.2.2 Quartz cell (1cm).
2.1.3 Test method
Measure the absorbance (A) of solution B at wavelength 455±1nm and wavelength 483±1nm. The ratio of As/Aas should be between 1.14 and 1.18.
Measure the absorbance (A) of solution B at wavelength 455±1nm and the absorbance (A) of solution A at wavelength 340±1nm. The ratio of Ass×10/A4 should not be less than 15. 2.2 Content determination
Principle: β-carotene is a conjugated double bond compound with maximum absorption at wavelength 455±1nm. The absorbance of the sample solution is measured at this wavelength, and the percentage content is calculated using the standard percentage absorption coefficient (Elem). 2.2.1 Reagents and solutions
2.2.1.1 Cyclohexane.
2.2.1.2 Chloroform (GB682-78).
2.2.1.3 Sample solution preparation: refer to 2.1.1.3 Solution B. 2.2.2 Instruments and equipment
2.2.2.1 UV spectrophotometer.
2.2.2.2 Quartz cell (1 cm).
2.2.3 Test method
Take solution B and use a suitable UV spectrophotometer to measure the absorbance (A) at a wavelength of 455±1 nm in a 1 cm quartz cell. Use cyclohexane as a blank control.
2.2.4 Calculation of analysis results:
-Percentage of β-carotene in the sample; Where:
A-absorbance reading of sample solution
W Mass of sample, g
V Total volume of sample dilution, mL;
V,——Volume of sample solution absorbed for determination, mL; 2500-Percentage absorption coefficient of β-carotene standard (Elem). 2.3 Melting point determination
2.3.1 Instruments and equipment
High beaker: 400mL.
(1)
Thermometer: graduation value 0.5℃.
GB8821—88
Capillary: inner diameter about 1mm, tube wall thickness about 0.15mm, length about 100mm. 2.3.2 Test method
Put a small amount of dry and finely ground sample (powdered sample can be directly put into a tube) into a clean and dry capillary with one end sealed. Take a dry glass tube about 800mm long, stand it upright on a porcelain plate or glass plate, and drop the capillary containing the sample 5 to 6 times until the sample in the capillary is shrunk to 23mm high. Add 300mL of silicone oil or glycerin as a temperature transfer liquid in a tall beaker, fix the thermometer in the middle of the temperature transfer liquid, heat the beaker, and stir continuously until the temperature rises slowly to 10℃ before the melting point. Attach the capillary containing the sample to the thermometer so that the sample layer and the middle of the mercury ball of the thermometer are at the same height, continue heating, and adjust the heating rate so that the temperature rises by 2.5 to 3℃ per minute. The temperature when the sample is partially liquefied is the initial melting temperature, and the temperature when the sample is completely liquefied is the full melting temperature. 2.3.3 Calibration
The thermometer is calibrated with a reference sample.
2.4. Salt determination
Principle: In a strong acid solution, the arsenic in the sample can be reduced to arsenic hydrogen by metallic zinc, and arsenic hydrogen reacts with mercuric bromide test paper to form a brown-yellow compound, namely arsenic spots. And compare the spots obtained by treating the arsenic standard solution in the same way to check the limit of arsenic salt in the sample.
2.4.1 Reagents and solutions
2.4.1.1 Dioxide (GB673-65). 2.4.1.2 Sodium hydroxide (GB62981) solution (5% solution). 2.4.1.3 Dilute sulfuric acid (GB625-77) (10% solution) Take 57mL of sulfuric acid and dilute it to 1000mL with water. 2.4.1.4 Hydrochloric acid (GB622-77).
2.4.1.5 Potassium iodide (GB1272-77) solution: Take 16.5g potassium iodide and add distilled water to dissolve into 100mL. 2.4.1.6 Acidic stannous fluoride solution: Take 20g stannous chloride and add hydrochloric acid to dissolve into 50mL, filter and obtain. This solution is not suitable for use three months after preparation.
2.4.1.7 Arsenic-free metallic zinc (GB230480). 30% hydrogen peroxide (HG3-1082-77). 2.4.1.8
2.4.1.9 Mercuric bromide (GB1398-78) test paper: Take a filter paper strip and immerse it in ethanol-based mercuric bromide test solution, take it out after 1 hour, and dry it in a dark place.
2.4.1.10 Preparation of arsenic standard solution
Accurately weigh 0.132g of arsenic trioxide dried to constant weight at 105℃, place in a 1000mL volumetric flask, add 5mL of sodium hydroxide solution (1→5) to dissolve, neutralize with an appropriate amount of dilute sulfuric acid, add 10mL of dilute sulfuric acid, dilute to scale with water, shake well, and use as stock solution. Before use, accurately measure 10mL of stock solution, place in a 1000mL volumetric flask, add 10mL of dilute sulfuric acid, dilute to scale with water, shake well, and the solution is obtained (each 1mL is equivalent to 1ug of arsenic). 2.4.1.11 Lead acetate (HG3-974-76) cotton: Take 1g of absorbent cotton and immerse it in 12mL of an equal volume mixture of lead acetate test solution and water. After it is soaked, squeeze to remove excess solution and make it loose. After drying below 100℃, store it in a glass stopper bottle for later use. 2.4.1.12 Preparation of standard arsenic spots: accurately measure 2 mL of arsenic standard solution and place it in bottle A, add 5 mL of hydrochloric acid and 21 mL of water, then add 5 mL of potassium iodide solution and 5 drops of acidic stannous chloride solution. After leaving it at room temperature for 10 minutes, add 2 g of zinc particles, and immediately plug the gas guide tube C installed according to the figure on bottle A, and place bottle A in a water bath at 25-40℃. After reacting for 1 hour, take out the mercuric bromide test paper, and you have it. 2.4.2 The instrument is as shown in the figure:
A is a 100mL standard ground-mouth conical flask.
B is a hollow standard ground-mouth stopper.
GB8821-88
C is an airway tube (outer diameter 8.0mm, inner diameter 6.0mm, total length about 180mm). D is a perforated organic glass stopper, the upper part of which is a circular plane with a circular hole in the center. The aperture is consistent with the inner diameter of the airway tube C, and the lower aperture is adapted to the outer diameter of the airway tube C. The top of the airway tube is inserted into the lower hole of the stopper, and the tube wall is matched with the circular hole of the stopper, and fixed by bonding.
E is an organic glass stopper cap with a circular hole in the center (aperture 6.0mm), which fits tightly with D. F is lead acetate cotton.
During the test, put 0.1g of lead acetate cotton in the airway C (the height of the tube is about 80mm), and then put a piece of mercuric bromide test paper on the top plane of the stopcock D (the size of the test paper should be able to cover the aperture without being exposed outside the plane), cover the stopcock cover E and tighten it, and you are done. 2.4.3 Test method
Weigh 1g of the sample into a 250mL conical flask, add 5mL of sulfuric acid, mix well, and slowly heat on an electric hot plate in a fume hood (not exceeding 120℃) until carbonization begins (the amount of sulfuric acid should not exceed 10mL). And carefully add 30% hydrogen peroxide solution, heat (250300℃) until the organic matter is completely destroyed, the white smoke is gone, and the solution becomes clear (almost colorless). After cooling, carefully add 10mL of water, evaporate to dryness, and let cool. Carefully add 10mL of water to clean the beaker, and transfer the solution to the arsenic bottle, add water to a total volume of 35mL, and follow the preparation of the standard monument spot, starting from adding 5mL of potassium iodide solution, and operate according to the law. Compare the generated arsenic spot with the standard spot, and it shall not be deeper. 2.5 Heavy Metal Determination
Principle: Use the impurity metals in the sample to develop color with hydrogen sulfide or sodium sulfide test solution under experimental conditions. And compare it with the standard lead solution in the same way. This is used to check the limit of heavy metals in the sample. 2.5.1 Reagents and Solutions
2.5.1.1 Nitric Acid (GB626-78).
2.5.1.2 Lead Nitrate (HG3-1070-77). 2.5.1.3 Dilute Acetic Acid (GB676-78) (6% Solution). Ammonia (GB631-77) (40% Solution). 2.5.1.4
2.5.1.5 Preparation of hydrogen sulfide solution
Pass hydrogen sulfide gas into water without carbon dioxide at room temperature until saturated. This solution should be placed in a brown bottle and stored in a cold place. 2.5.1.6 Preparation of lead standard solution
GB8821-88
Accurately weigh 0.159.8g of lead nitrate dried to constant weight at 105℃, place it in a 1000mL volumetric flask, add 1mL of nitric acid and 100mL of water to dissolve, dilute with water to the scale, shake well, and use as the stock solution. Before use, accurately measure 10mL of the stock solution, place it in a 100mL volumetric flask, dilute with water to the scale, shake well, and obtain (each 1mL is equivalent to 10 μg of Pb).
2.5.2 Test method
Take 2.0g of sample and place it in a suitable crucible. Add enough sulfuric acid to wet the sample and slowly ignite until it is completely carbonized. Add 2mL nitric acid and 5 drops of sulfuric acid. Heat at low temperature until sulfuric acid vapor is completely removed. Then ignite at 500-600℃ to completely carbonize it. Let it cool. Add 4mL of dilute hydrochloric acid (1:2). Heat it in a water bath for 10-15min and evaporate it to dryness. Wet the residue with a drop of hydrochloric acid. Add 10mL of hot water and warm it for 2min. Add ammonia test solution until it is alkaline to litmus paper. Dilute it to 25mL with water and adjust the pH to 3.0-4.0 with dilute acetic acid. Take another test tube, add 2mL of lead standard solution and 2mL of dilute acetic acid, dilute with water to 25mL, add 10mL of hydrogen sulfide solution to each tube, shake well, place in a dark place for 10min, place on white paper, and see through from above. The color of the sample should not be darker than that of the lead standard solution tube. 2.6 Determination of ignition residue
Principle: The sulfate remaining after the sample is ignited with sulfuric acid is determined by weight. 2.6.1 Reagents and solutions
Dilute sulfuric acid (GB625-77) is the same as 2.4.1.3.
2.6.2 Instruments and equipment
2.6.2.1 Quartz crucible (diameter about 37mm, height about 48mm). 2.6.2.2 High temperature furnace.
2.6.3 Test method
Accurately weigh about 2g of the sample and place it in a flaming furnace until constant weight is reached. Add dilute sulfuric acid to completely wet the sample, and then slowly flaming until it is completely carbonized. Then add 0.1mL of sulfuric acid to wet it, heat it at low temperature until sulfuric acid vapor is completely removed, and then flaming it at 800±25℃ to completely ash it. Move it to a desiccator, cool it, accurately weigh it, and flaming it again until constant weight is reached. 2.6.4 Calculation of analysis results
Where: - sample flaming residue, expressed as mass percentage; G. Total mass of crucible and ash, g;
G, - crucible mass, g;
G - sample mass, g.
2.7 Dissolution test
2.7.1 Reagents
Trichloromethane (GB682-78).
2.7.2 Test method
Accurately weigh about 1g of sample and dissolve it in 100mL of chloroform. The solution should be clear. 3 Acceptance rules
·(2)
3.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer guarantees that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory should be accompanied by a product quality certificate. 3.2 The user unit can conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
3.3 Sampling method
1% of the sample should be selected from each batch of packaging. Use the sampling tool to reach into the depth of three-quarters of the sample to take a sufficient amount of sample, place it in a clean, dry, airtight and light-proof sealed container, affix a label, indicate the manufacturer name, product name, batch number and sampling date, cool it in a dry place, and test it in time.
GB8821—88
3.4 If one of the indicators does not meet the standard requirements during the inspection, re-sampling should be carried out for re-inspection. If even one of the indicators does not meet the standard, the whole batch of products cannot be accepted. 3.5 If the supply and demand parties have objections to the product quality, they can ask the arbitration unit to conduct arbitration inspection in accordance with the inspection rules and methods specified in this standard.
4 Marking, packaging, transportation and storage
4.1 Marking
The product name, batch number, net weight, approval number, manufacturer name and storage requirements should be written on the label. And indicate: "Food additives", the original packaging has a shelf life of one year.
4.2 Packaging
β-carotene is packed in a light-proof sealed container, which needs to be filled with nitrogen or vacuumed after packaging. This product should be used as soon as possible after opening to avoid oxidation, heat, moisture and deterioration.
4.3 Transportation
This product must not be mixed or transported with toxic, harmful or other contaminated items and oxidizing items. 4.4 Storage
β-Carotene crystals are easy to oxidize and should be stored in a dark, cold and dry place to prevent heat and moisture. Additional remarks:
This standard was proposed by the State Drug Administration and the Ministry of Health of the People's Republic of China. This standard is technically managed by the China Pharmaceutical Industry Corporation of the State Drug Administration and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai No. 6 Pharmaceutical Factory, Shanghai Food Hygiene Supervision and Inspection Institute, and Beijing Pharmaceutical Industry Research Institute.3 Test method
Weigh 1g of sample into a 250mL conical flask, add 5mL of sulfuric acid, mix well, and slowly heat on an electric hot plate in a fume hood (not exceeding 120℃) until carbonization begins (the amount of sulfuric acid should not exceed 10mL). Carefully add 30% hydrogen peroxide solution and heat (250300℃) until the organic matter is completely destroyed, the white smoke is gone, and the solution becomes clear (almost colorless). After cooling, carefully add 10mL of water, evaporate to dryness, and let cool. Carefully add 10mL of water to clean the beaker, and transfer the solution to the arsenic bottle, adding water to a total volume of 35mL. According to the preparation of the standard monument spot, start from adding 5mL of potassium iodide solution and operate according to the law. Compare the generated arsenic spot with the standard spot, which shall not be deeper. 2.5 Heavy metal determination
Principle: Use the impurity metals in the sample to develop color with hydrogen sulfide or sodium sulfide test solution under test conditions. And compare it with the standard lead solution in the same way. This is used to check the limit of heavy metals in the sample. 2.5.1 Reagents and solutions
2.5.1.1 Nitric acid (GB626-78).
2.5.1.2 Lead nitrate (HG3-1070-77). 2.5.1.3 Dilute acetic acid (GB676-78) (6% solution). Ammonia water (GB631-77) (40% solution). 2.5.1.4
2.5.1.5 Preparation of hydrogen sulfide solution
Pass hydrogen sulfide gas into water without carbon dioxide at room temperature until it is saturated. This solution should be placed in a brown bottle and stored in a cold place. 2.5.1.6 Preparation of lead standard solution
GB8821-88
Accurately weigh 0.159.8g of lead nitrate dried to constant weight at 105℃, place in a 1000mL volumetric flask, add 1mL of nitric acid and 100mL of water to dissolve, dilute to scale with water, shake well, and use as stock solution. Before use, accurately measure 10mL of stock solution, place in a 100mL volumetric flask, dilute to scale with water, shake well, and obtain (each 1mL is equivalent to 10 μg of Pb).
2.5.2 Test method
Take 2.0g of sample and place in a suitable crucible, add sufficient sulfuric acid to wet the sample, and slowly ignite until it is completely carbonized. Add 2mL nitric acid and 5 drops of sulfuric acid, heat at low temperature until sulfuric acid vapor is completely removed, ignite at 500-600℃ to completely carbonize, cool, add 4mL dilute hydrochloric acid (1:2), heat in a water bath for 10-15min and evaporate to dryness, moisten the residue with a drop of hydrochloric acid, add 10mL hot water and warm for 2min, add ammonia test solution until it is alkaline to litmus paper. Dilute with water to 25mL, and adjust the pH to 3.0-4.0 with dilute acetic acid. Take another test tube, add 2mL of lead standard solution and 2mL of dilute acetic acid, dilute with water to 25mL, add 10mL of hydrogen sulfide solution to each tube, shake well, place in a dark place for 10min, place on white paper, and see through from above. The color of the sample should not be darker than that of the lead standard solution tube. 2.6 Determination of ignition residue
Principle: The sulfate remaining after the sample is ignited with sulfuric acid is determined by weight. 2.6.1 Reagents and solutions
Dilute sulfuric acid (GB625-77) is the same as 2.4.1.3.
2.6.2 Apparatus
2.6.2.1 Quartz crucible (diameter about 37mm, height about 48mm). 2.6.2.2 High temperature furnace.
2.6.3 Test method
Accurately weigh about 2g of sample and place it in a furnace that is incinerated to constant weight. Add dilute sulfuric acid to completely wet the sample, and then slowly incinerate until it is completely carbonized. Then add 0.1mL of sulfuric acid to wet it, heat at low temperature until sulfuric acid vapor is completely removed, and incinerate at 800±25℃ to completely ash it. Transfer it to a desiccator, cool it, accurately weigh it, and incinerate it again to constant weight to obtain the sample. 2.6.4 Calculation of analysis results
Where: - sample ignition residue, expressed as mass percentage; G. Total mass of crucible and ash, g;
G, — mass of crucible, g;
G — mass of sample, g.
2.7 Dissolution test
2.7.1 Reagents
Chloroform (GB682-78).
2.7.2 Test method
Accurately weigh about 1g of sample and dissolve it in 100mL of chloroform. The solution should be clear. 3 Acceptance rules
· (2)
3.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer guarantees that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory should be accompanied by a product quality certificate. 3.2 The user unit can conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
3.3 Sampling method
1% of the samples should be selected from each batch of packaging, and the sampling tool should be inserted into the sample to three-quarters of the depth, and a sufficient amount of samples should be placed in a clean, dry, airtight and light-proof sealed container. A label should be attached, indicating the manufacturer's name, product name, batch number and sampling date, and refrigerated in a dry place, and tested in time.
GB8821—88
3.4 If one of the indicators does not meet the standard requirements during the inspection, re-sampling should be carried out for re-inspection. If even one of the indicators of the product does not meet the requirements of this standard, the entire batch of products cannot be accepted. 3.5 If the supply and demand parties have objections to the product quality, the two parties may request the arbitration unit to conduct arbitration inspection in accordance with the inspection rules and methods specified in this standard.
4 Labeling, packaging, transportation and storage
4.1 Labeling
The product name, batch number, net weight, approval number, manufacturer name and storage requirements should be clearly stated on the label. And the words "food additive" should be noted. The shelf life of the original packaging is one year.
4.2 Packaging
β-carotene should be packed in a light-proof and airtight container. After packing, it needs to be filled with nitrogen or vacuumed. This product should be used as soon as possible after opening to avoid oxidation, heat, moisture and deterioration.
4.3 Transportation
This product shall not be mixed or transported with toxic, harmful or other contaminated items and oxidizing items. 4.4 Storage
β-carotene crystals are more easily oxidized and should be stored in a light-proof, cold and dry place to prevent heat and moisture. Additional remarks:
This standard was proposed by the State Food and Drug Administration and the Ministry of Health of the People's Republic of China. This standard is under the technical supervision of China Pharmaceutical Industry Corporation of the State Drug Administration and the Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai No. 6 Pharmaceutical Factory, Shanghai Food Sanitation Supervision and Inspection Institute, and Beijing Pharmaceutical Industry Research Institute.3 Test method www.bzxz.net
Weigh 1g of sample into a 250mL conical flask, add 5mL of sulfuric acid, mix well, and slowly heat on an electric hot plate in a fume hood (not exceeding 120℃) until carbonization begins (the amount of sulfuric acid should not exceed 10mL). Carefully add 30% hydrogen peroxide solution and heat (250300℃) until the organic matter is completely destroyed, the white smoke is gone, and the solution becomes clear (almost colorless). After cooling, carefully add 10mL of water, evaporate to dryness, and let cool. Carefully add 10mL of water to clean the beaker, and transfer the solution to the arsenic bottle, adding water to a total volume of 35mL. According to the preparation of the standard monument spot, start from adding 5mL of potassium iodide solution and operate according to the law. Compare the generated arsenic spot with the standard spot, which shall not be deeper. 2.5 Heavy metal determination
Principle: Use the impurity metals in the sample to develop color with hydrogen sulfide or sodium sulfide test solution under test conditions. And compare it with the standard lead solution in the same way. This is used to check the limit of heavy metals in the sample. 2.5.1 Reagents and solutions
2.5.1.1 Nitric acid (GB626-78).
2.5.1.2 Lead nitrate (HG3-1070-77). 2.5.1.3 Dilute acetic acid (GB676-78) (6% solution). Ammonia water (GB631-77) (40% solution). 2.5.1.4
2.5.1.5 Preparation of hydrogen sulfide solution
Pass hydrogen sulfide gas into water without carbon dioxide at room temperature until it is saturated. This solution should be placed in a brown bottle and stored in a cold place. 2.5.1.6 Preparation of lead standard solution
GB8821-88
Accurately weigh 0.159.8g of lead nitrate dried to constant weight at 105℃, place in a 1000mL volumetric flask, add 1mL of nitric acid and 100mL of water to dissolve, dilute to scale with water, shake well, and use as stock solution. Before use, accurately measure 10mL of stock solution, place in a 100mL volumetric flask, dilute to scale with water, shake well, and obtain (each 1mL is equivalent to 10 μg of Pb).
2.5.2 Test method
Take 2.0g of sample and place in a suitable crucible, add sufficient sulfuric acid to wet the sample, and slowly ignite until it is completely carbonized. Add 2mL nitric acid and 5 drops of sulfuric acid, heat at low temperature until sulfuric acid vapor is completely removed, ignite at 500-600℃ to completely carbonize, cool, add 4mL dilute hydrochloric acid (1:2), heat in a water bath for 10-15min and evaporate to dryness, moisten the residue with a drop of hydrochloric acid, add 10mL hot water and warm for 2min, add ammonia test solution until it is alkaline to litmus paper. Dilute with water to 25mL, and adjust the pH to 3.0-4.0 with dilute acetic acid. Take another test tube, add 2mL of lead standard solution and 2mL of dilute acetic acid, dilute with water to 25mL, add 10mL of hydrogen sulfide solution to each tube, shake well, place in a dark place for 10min, place on white paper, and see through from above. The color of the sample should not be darker than that of the lead standard solution tube. 2.6 Determination of ignition residue
Principle: The sulfate remaining after the sample is ignited with sulfuric acid is determined by weight. 2.6.1 Reagents and solutions
Dilute sulfuric acid (GB625-77) Same as 2.4.1.3.
2.6.2 Apparatus
2.6.2.1 Quartz crucible (diameter about 37mm, height about 48mm). 2.6.2.2 High temperature furnace.
2.6.3 Test method
Accurately weigh about 2g of sample and place it in a furnace that is incinerated to constant weight. Add dilute sulfuric acid to completely wet the sample, and then slowly incinerate until it is completely carbonized. Then add 0.1mL of sulfuric acid to wet it, heat at low temperature until sulfuric acid vapor is completely removed, and incinerate at 800±25℃ to completely ash it. Transfer it to a desiccator, cool it, accurately weigh it, and incinerate it again to constant weight to obtain the sample. 2.6.4 Calculation of analysis results
Where: - sample ignition residue, expressed as mass percentage; G. Total mass of crucible and ash, g;
G, — mass of crucible, g;
G — mass of sample, g.
2.7 Dissolution test
2.7.1 Reagents
Chloroform (GB682-78).
2.7.2 Test method
Accurately weigh about 1g of sample and dissolve it in 100mL of chloroform. The solution should be clear. 3 Acceptance rules
· (2)
3.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer guarantees that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory should be accompanied by a product quality certificate. 3.2 The user unit can conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
3.3 Sampling method
1% of the samples should be selected from each batch of packaging, and the sampling tool should be inserted into the sample to three-quarters of the depth, and a sufficient amount of samples should be placed in a clean, dry, airtight and light-proof sealed container. A label should be attached, indicating the manufacturer's name, product name, batch number and sampling date, and refrigerated in a dry place, and tested in time.
GB8821—88
3.4 If one of the indicators does not meet the standard requirements during the inspection, re-sampling should be carried out for re-inspection. If even one of the indicators of the product does not meet the requirements of this standard, the entire batch of products cannot be accepted. 3.5 If the supply and demand parties have objections to the product quality, the two parties may request the arbitration unit to conduct arbitration inspection in accordance with the inspection rules and methods specified in this standard.
4 Labeling, packaging, transportation and storage
4.1 Labeling
The product name, batch number, net weight, approval number, manufacturer name and storage requirements should be clearly stated on the label. And the words "food additive" should be noted. The shelf life of the original packaging is one year.
4.2 Packaging
β-carotene should be packed in a light-proof and airtight container. After packing, it needs to be filled with nitrogen or vacuumed. This product should be used as soon as possible after opening to avoid oxidation, heat, moisture and deterioration.
4.3 Transportation
This product shall not be mixed or transported with toxic, harmful or other contaminated items and oxidizing items. 4.4 Storage
β-carotene crystals are more easily oxidized and should be stored in a light-proof, cold and dry place to prevent heat and moisture. Additional remarks:
This standard was proposed by the State Food and Drug Administration and the Ministry of Health of the People's Republic of China. This standard is under the technical supervision of China Pharmaceutical Industry Corporation of the State Drug Administration and the Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai No. 6 Pharmaceutical Factory, Shanghai Food Sanitation Supervision and Inspection Institute, and Beijing Pharmaceutical Industry Research Institute.6 Determination of ignition residue
Principle: The sulfate remaining after the sample is ignited with sulfuric acid is determined by weight. 2.6.1 Reagents and solutions
Dilute sulfuric acid (GB625-77) is the same as 2.4.1.3.
2.6.2 Instruments and equipment
2.6.2.1 Quartz crucible (diameter about 37mm, height about 48mm). 2.6.2.2 High temperature furnace.
2.6.3 Test method
Accurately weigh about 2g of the sample and place it in a furnace that is ignited to constant weight. Add dilute sulfuric acid to completely wet the sample, and then slowly ignite it until it is completely carbonized. Then add 0.1mL of sulfuric acid to wet it, heat it at low temperature until the sulfuric acid vapor is completely removed, and ignite it at 800±25℃ to completely ash it. Move it to a desiccator, let it cool, accurately weigh it, and ignite it again to constant weight to obtain the result. 2.6.4 Calculation of analysis results
Where: - sample ignition residue, expressed as mass percentage; G. Total mass of crucible and ash, g;
G, — mass of crucible, g;
G — mass of sample, g.
2.7 Dissolution test
2.7.1 Reagents
Chloroform (GB682-78).
2.7.2 Test method
Accurately weigh about 1g of sample and dissolve it in 100mL of chloroform. The solution should be clear. 3 Acceptance rules
· (2)
3.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer guarantees that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory should be accompanied by a product quality certificate. 3.2 The user unit can conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
3.3 Sampling method
1% of the samples should be selected from each batch of packaging, and the sampling tool should be inserted into the sample to three-quarters of the depth, and a sufficient amount of samples should be placed in a clean, dry, airtight and light-proof sealed container. A label should be attached, indicating the manufacturer's name, product name, batch number and sampling date, and refrigerated in a dry place, and tested in time.
GB8821—88
3.4 If one of the indicators does not meet the standard requirements during the inspection, re-sampling should be carried out for re-inspection. If even one of the indicators of the product does not meet the requirements of this standard, the entire batch of products cannot be accepted. 3.5 If the supply and demand parties have objections to the product quality, the two parties may request the arbitration unit to conduct arbitration inspection in accordance with the inspection rules and methods specified in this standard.
4 Labeling, packaging, transportation and storage
4.1 Labeling
The product name, batch number, net weight, approval number, manufacturer name and storage requirements should be clearly stated on the label. And the words "food additive" should be noted. The shelf life of the original packaging is one year.
4.2 Packaging
β-carotene should be packed in a light-proof and airtight container. After packing, it needs to be filled with nitrogen or vacuumed. This product should be used as soon as possible after opening to avoid oxidation, heat, moisture and deterioration.
4.3 Transportation
This product shall not be mixed or transported with toxic, harmful or other contaminated items and oxidizing items. 4.4 Storage
β-carotene crystals are more easily oxidized and should be stored in a light-proof, cold and dry place to prevent heat and moisture. Additional remarks:
This standard was proposed by the State Food and Drug Administration and the Ministry of Health of the People's Republic of China. This standard is under the technical supervision of China Pharmaceutical Industry Corporation of the State Drug Administration and the Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai No. 6 Pharmaceutical Factory, Shanghai Food Sanitation Supervision and Inspection Institute, and Beijing Pharmaceutical Industry Research Institute.6 Determination of ignition residue
Principle: The sulfate remaining after the sample is ignited with sulfuric acid is determined by weight. 2.6.1 Reagents and solutions
Dilute sulfuric acid (GB625-77) is the same as 2.4.1.3.
2.6.2 Instruments and equipment
2.6.2.1 Quartz crucible (diameter about 37mm, height about 48mm). 2.6.2.2 High temperature furnace.
2.6.3 Test method
Accurately weigh about 2g of the sample and place it in a furnace that is ignited to constant weight. Add dilute sulfuric acid to completely wet the sample, and then slowly ignite it until it is completely carbonized. Then add 0.1mL of sulfuric acid to wet it, heat it at low temperature until the sulfuric acid vapor is completely removed, and ignite it at 800±25℃ to completely ash it. Move it to a desiccator, let it cool, accurately weigh it, and ignite it again to constant weight to obtain the result. 2.6.4 Calculation of analysis results
Where: - sample ignition residue, expressed as mass percentage; G. Total mass of crucible and ash, g;
G, — mass of crucible, g;
G — mass of sample, g.
2.7 Dissolution test
2.7.1 Reagents
Chloroform (GB682-78).
2.7.2 Test method
Accurately weigh about 1g of sample and dissolve it in 100mL of chloroform. The solution should be clear. 3 Acceptance rules
· (2)
3.1 This product should be inspected by the quality inspection department of the manufacturer. The manufacturer guarantees that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory should be accompanied by a product quality certificate. 3.2 The user unit can conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
3.3 Sampling method
1% of the samples should be selected from each batch of packaging, and the sampling tool should be inserted into the sample to three-quarters of the depth, and a sufficient amount of samples should be placed in a clean, dry, airtight and light-proof sealed container. A label should be attached, indicating the manufacturer's name, product name, batch number and sampling date, and refrigerated in a dry place, and tested in time.
GB8821—88
3.4 If one of the indicators does not meet the standard requirements during the inspection, re-sampling should be carried out for re-inspection. If even one of the indicators of the product does not meet the requirements of this standard, the entire batch of products cannot be accepted. 3.5 If the supply and demand parties have objections to the product quality, the two parties may request the arbitration unit to conduct arbitration inspection in accordance with the inspection rules and methods specified in this standard.
4 Labeling, packaging, transportation and storage
4.1 Labeling
The product name, batch number, net weight, approval number, manufacturer name and storage requirements should be clearly stated on the label. And the words "food additive" should be noted. The shelf life of the original packaging is one year.
4.2 Packaging
β-carotene should be packed in a light-proof and airtight container. After packing, it needs to be filled with nitrogen or vacuumed. This product should be used as soon as possible after opening to avoid oxidation, heat, moisture and deterioration.
4.3 Transportation
This product shall not be mixed or transported with toxic, harmful or other contaminated items and oxidizing items. 4.4 Storage
β-carotene crystals are more easily oxidized and should be stored in a light-proof, cold and dry place to prevent heat and moisture. Additional remarks:
This standard was proposed by the State Food and Drug Administration and the Ministry of Health of the People's Republic of China. This standard is under the technical supervision of China Pharmaceutical Industry Corporation of the State Drug Administration and the Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Shanghai No. 6 Pharmaceutical Factory, Shanghai Food Sanitation Supervision and Inspection Institute, and Beijing Pharmaceutical Industry Research Institute.
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