Some standard content:
GB16314—1996
L-Ascorbyl palmitate is a food additive. It was once widely used as an antioxidant in various foods abroad. Since this product is a derivative of vitamin C (ascorbic acid), it can provide vitamin C for the body, so it can also be used as a nutritional enhancer. This standard is not equivalent to the standard of ascorbic acid hexadecyl ester in the third edition of the "Food Chemical Codex of the United States" in 1983 (FCC1 for short) (it was found that the fourth supplementary edition of FCC in 1994 was not revised). Iodine titration is added under the identification item. Some items in the test method are the same as FCC, and some items are different from FCCⅡ. It is mainly to be consistent with the national standard and the test method is more reasonable. However, its principles and results are equivalent.
This standard is proposed by the State Drug Administration. This standard is organized and drafted by China Pharmaceutical Industry Corporation and technically managed by Tianjin Pharmaceutical Research Institute. The drafting unit of this standard is: Shijiazhuang No. 1 Pharmaceutical Factory, Hebei Province. The main drafters of this standard are: Che Yingcheng, Zhong Nanping, and Yuan Hongzhong. 295
National Standard of the People's Republic of China
Food additive
L-ascorbyl palmitate
Food additive
-L-ascorbyl palmitate
GB16314-1996
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage requirements of the food additive L-ascorbyl palmitate.
This standard applies to L-ascorbyl palmitate prepared by reacting palmitic acid with thionyl chloride to prepare palmitic acid, which is then reacted with L-ascorbic acid. It can be added to food as an antioxidant and a nutritional enhancer for supplementing vitamin C. Cited standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest version of the following standards. GB60188 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB 602-88
GB 603-88
GB 613--88
Preparation of standard solutions for determination of impurities in chemical reagents Preparation of preparations and products used in test methods for chemical reagents General method for determination of specific rotation of chemical reagents GB8450-87 Determination of impurities in food additives GB8451-87 Test method for limits of heavy metals in food additives Pharmacopoeia of the People's Republic of China, 1995 edition (Part II) 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name; I-ascorbic acid + hexadecanoate
L-ascorbic acid, 6-hexadecanoate Molecular formula: C2H38O,
Structural formula:
CH3(CH2 )1,COOCH2
Molecular weight: 414.54 (according to the international atomic weight of 1987) 4 Technical requirements
4.1 Properties
Approved by the State Bureau of Technical Supervision on May 21, 1996296
Implementation on December 1, 1996
GB16314---1996
This product is a white or yellow powder with a slight odor. It is very slightly soluble in water and vegetable oil, and easily soluble in anhydrous ethanol and anhydrous methanol. At room temperature, 4.5mL of anhydrous ethanol can dissolve 1g of this product, and its solubility increases with increasing temperature. 4.2 Items and indicators
Content (as C22H3g0), %
Specific rotation [αJ
Melting point range, ℃
Loss on drying, %
Ignition residue, %
Arsenic salt (as As), %
Heavy metal (as Pb), %
Test method
+21°～+24°
107～117
Unless otherwise specified, the reagents used in the test are all analytically pure reagents; water is distilled water or water of corresponding purity; instruments and equipment are general laboratory instruments and equipment.
5.1 Identification
5.1.1 Principle
The sodium dichloroindophenol solution and iodine solution test is based on the fact that this product contains an enediol structure in its structure. Sodium or iodine is oxidized to a diketone structure
5.1.2 Reagents and solutions
, which is easily oxidized to dichloroindophenol
, and the sodium dichloroindophenol solution or iodine solution test fades. Based on this, this product can be identified. 5.1.2.1 2,6-Sodium dichloroindophenol solution: 0.1% (m/V) aqueous solution. 5.1.2.2 Anhydrous ethanol (GB678).
5.1.2.3 Iodine solution: 0.1mol/L (GB675). 5.1.3 Identification method
5.1.3.1 Dissolve 1g of this product in 10mL of anhydrous ethanol. This solution can decolorize 0.1% 2,6-dichloroindophenol sodium aqueous solution. 5.1.3.2 Dissolve 1g of this product in 10mL of anhydrous ethanol. This solution can decolorize 0.1mol/L iodine solution. 5.2 Content determination
5.2.1 Principle
Use iodine titration method. This product contains enediol structure and keto structure in its structure. At the same time, iodine is reduced to generate HI.
5.2.2 Reagents and solutions
, which has strong reducing properties and is easily oxidized to dihydrogen by iodine solution. 5.2.2.1 Iodine standard titration solution (0.1mol/L): Weigh an appropriate amount of iodine (GB675) and prepare it according to the method specified in GB603. 5.2.2.2 Anhydrous ethanol (GB 678).
5.2.3 Determination methodbZxz.net
GB16314-1996
Weigh about 0.3g of sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask, add 50mL of anhydrous ethanol to dissolve it, then add 30mL of water, shake well, and immediately titrate with 0.1mol/L iodine standard solution until it turns yellow. The end point is that it does not fade within 30s, and record the volume of iodine standard solution consumed (ml).
5.2.4 Calculation of results
The content of L-ascorbyl palmitate X, (%) is expressed as mass percentage and can be calculated according to formula (1): V: GX 0. 207 3
Wherein: V--
The volume of iodine standard titrant consumed by titrating the sample, mL; the concentration of iodine standard titrant, mol/L, - the mass of the weighed sample, g;
(1)
0.2073--The mass of L-ascorbyl palmitate in grams equivalent to 1.00mL iodine standard titrant c(1/21,)=1.000mol/1.],
Take the arithmetic mean of the two calculations as the test result, which should be expressed to one decimal place. 5.2.5 Allowable error
The allowable relative deviation of the two parallel determinations of this method is within 0.3%. 5.3 Determination of specific rotation
5.3.1 Instrument and reagents
5.3.1.1 Instrument: Use the instrument specified in GB613. 5.3.1.2 Reagent: Methanol (GB683).
5.3.2 Determination method
Weigh about 2g of sample (accurate to 0.002g), place in a 20mL volumetric flask, add methanol to dissolve and dilute to the scale, shake well, operate according to the method specified in GB613, and adjust the temperature to 25℃±0.5℃, and determine. 5.3.3 Explanation of results
Specific rotation [α] is calculated according to formula (2):
——Specific rotation at 25℃;
Where: [α
α——Optical rotation measured at 25℃; 1——Length of the polarimetric tube, dm,
[a = × 100
The mass of L-ascorbyl palmitate in 100mlL solution (calculated on the basis of dry product), g. 5.4 Determination of melting point range
Determine according to the first method of melting point determination on page 33 of Appendix II of the 1995 edition of the Pharmacopoeia of the People's Republic of China. --.( 2)
5.5 Determination of loss on drying
Grind about 1g of sample into particles of about 2mm in size, place in a weighed flat weighing bottle that has been dried for 30min under the same conditions as the sample determination, weigh accurately, then place the sample bottle in a vacuum drying oven, dry at 56℃～60℃ and a pressure of about 2.67kPa (20mmHg) for 1h, take it out and cool it to room temperature in a desiccator, weigh it, and calculate the loss on drying from the lost weight and the sample amount. 5.6 Determination of ignition residue
5.6.1 Reagents and solutions
Sulfuric acid (GB 625).
5.6.2 Determination method
Weigh 1g of sample (weigh to 0.01g), placed in a porcelain crucible that has been burned to constant weight at 700℃～800℃, first slowly heated with low heat until completely carbonized, after cooling, add 0.5mL～1.0mL of sulfuric acid to make it moist, heat at low temperature until sulfuric acid vapor is completely removed, then transfer to a muffle furnace and burn to constant weight at 700℃～800℃. 298
5.6.3 Explanation of results
GB 16314—1996
The burning residue X, (%) is expressed as mass percentage and calculated according to formula (3): Xz = ms=m × 100
Where: m2——
-total mass of crucible and residue, g;
m3—mass of crucible + g
m4—mass of sample, g.
5.7 Determination of arsenic
Determine according to the wet digestion arsenic spot method in GB8450. 5.8 Determination of heavy metals
Determine according to the dry method in GB8451.
6 Inspection rules
(3)
6.1 This product shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all products shipped meet the requirements of the standard. Each product shall be accompanied by a product certificate.
6.2 The user may conduct quality inspection on the received products in accordance with this standard. 6.3 The sampling method shall be determined according to the number of packages. When the total number of packages n≤3, the sampling number is each package. When the total number of packages n≤300, the sampling number is /n+1. When the total number of packages n>300, the sampling number is /n+1. Use a clean and suitable sampler to penetrate three-quarters of the depth of each package. Each piece of equal amount is sampled, and 10 times the amount used for testing is sampled by quartering method, divided into two parts, and placed in clean, dry, airtight and light-proof sample bottles. The bottles are labeled with product name, batch number, manufacturer name and sampling date, signature of the sampler and necessary instructions. One copy is sent to the laboratory, and the other is sealed and kept for arbitration analysis. 6.4 If one of the indicators in the test results does not meet this standard, the number of samples should be doubled, and the samples should be re-tested. If one of the results of the re-test of the product does not meet the standard, the entire batch of products is unqualified. 6.5 If the supply and demand parties have objections to the product quality, the two parties can negotiate and select an arbitration unit to conduct arbitration in accordance with this standard. 7 Marking, packaging, transportation, storage
7.1 The packaging should have a firm mark, which should include: product name (marked with "food additives"), batch number, product production approval number, production date, net weight, trademark, manufacturer name, factory address and storage conditions. 7.2 This product should be packed in a cardboard barrel/box, lined with a kraft paper bag and a double-layer polyethylene plastic bag for food, with a pack of silica gel desiccant in the interlayer. The quantity per barrel/box is determined according to market requirements. 7.3 This product must not be mixed or transported with toxic, harmful or other polluting items and oxidizing substances. 7.4 This product should be stored in a dry place away from light and prevent moisture and heat. 7.5 Packed according to regulations, the shelf life of the original packaging is two years (use as soon as possible after opening to avoid deterioration). 299
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