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GB 23386-2017: Feed additive -- Vitamin A palmitate (powder form)
Status: Valid

GB 23386: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB 23386-2017279 Add to Cart 3 days Feed additive -- Vitamin A palmitate (powder form) Valid
GB/T 23386-2009319 Add to Cart 3 days Feed additive -- Vitamin A palmitate powder Obsolete

Similar standards

GB/T 23742   GB/T 23879   GB/T 23882   GB/T 23387   GB/T 23385   

Basic data

Standard ID: GB 23386-2017 (GB23386-2017)
Description (Translated English): Feed additive -- Vitamin A palmitate (powder form)
Sector / Industry: National Standard
Classification of Chinese Standard: B46
Classification of International Standard: 65.120
Word Count Estimation: 14,149
Date of Issue: 2017-10-14
Date of Implementation: 2018-05-01
Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China

GB 23386-2017: Feed additive -- Vitamin A palmitate (powder form)

---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.
Feed additive - Vitamin A palmitate (powder form) ICS 65.120 B46 National Standards of People's Republic of China Replacing GB/T 23386-2009 Feed Additives Vitamin A Palmitate (Powdered) 2017-10-14 Published 2018-05-01 implementation General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China China National Standardization Administration released

Foreword

The first chapter of this standard, Chapter 3 and Chapter 5 is mandatory, the rest are recommended. This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 23386-2009 "feed additive vitamin A palmitate powder." This standard compared with GB/T 23386-2009, the main technical differences are as follows. --- Product traits modified to "light yellow to yellow liquid particles or powder, no obvious odor, the air, heat, light and humidity sensitive"; --- Chapter 3 added "product specifications" requirements; --- Total arsenic by "≤ 3mg/kg" revised "≤ 2mg/kg"; --- Modify the determination of vitamin A palmitate content; --- Determination of particle size modified to GB/T 5917.1 provided for the implementation of the method; --- Added Appendix A This standard is proposed and managed by the National Feed Industry Standardization Technical Committee (SAC/TC76). This standard was drafted unit. New and into Zhejiang Co., Ltd., China Feed Industry Association, Zhejiang Pharmaceutical Co., Ltd., Zhejiang Province, animal Drug Feed Inspection Office. The main drafters of this standard. Yang Jinshu, Wang Liwen, Zhu Congying, Shi Dongming, Ren Yuqin, Zhang Xianghan, Yang Yahong, Ye Yueheng, Pan Dayong, Wang Wenfeng, Lu Weijun, Jiang Hongjun, Su Junfen. This standard replaces the standards previously issued as. --- GB/T 23386-2009. Feed Additives Vitamin A Palmitate (Powdered)

1 Scope

This standard specifies the feed additive Vitamin A palmitate (powder) product requirements, test methods, inspection rules and labels, packages Loading, transportation, storage and shelf life. This standard applies to chemical synthesis of vitamin A palmitate as raw material, modified starch and other accessories, adding the right amount of antioxidants to Spray process production of feed additives vitamin A palmitate (powder). Chemical name 3,7-Dimethyl-9- (2,6,6-trimethyl-1-cyclohexen-1-yl) -2,4,6,8-nonatetraene-1-palm Acid ester Molecular formula .C36H60O2 Relative molecular mass. 524. 86 (International relative atomic mass in.2007) Chemical Structure.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version applies to this article For all undated references, the latest edition (including all amendments) applies to this document. GB/T 601 chemical reagent standard titration solution preparation GB/T 603 chemical reagent test methods used in the preparation of preparations and products GB/T 5917.1 forage particle size determination two sieve screening method GB/T 6435 Determination of moisture in feed GB/T 6682 analytical laboratory water specifications and test methods GB 10648 feed label GB/T 14699.1 feed sampling

3 requirements

3.1 Appearance and traits This product is light yellow to yellow fluid particles or powder, no obvious odor, the air, heat, light and humidity sensitive. 3.2 Product Specifications 3.2.1 25 million IU/g. 3.2.2 Product specifications can also be determined according to the contract (but not less than 250,000 IU/g). 3.3 Technical Specifications Technical indicators should meet the requirements of Table 1. Table 1 technical indicators Project Indicators Vitamin A palmitate content (accounting for the amount) /% 95.0 ~ 115.0 Vitamin A alcohol and vitamin A acetate total content /% ≤ 1.0 granularity 100% through a 0.84mm aperture test sieve More than 85% through the aperture of 0.425mm test sieve Loss on drying /% ≤8.0 Heavy metals (Pb)/(mg/kg) ≤ 10 Total arsenic (As)/(mg/kg) ≤2

4 test methods

Unless otherwise specified, the reagents used are of analytical grade; the chromatographic and spectral analysis of water used are in line with GB/T 6682 in a water regulation Set, and other test water in line with the provisions of GB/T 6682 in the three water; reagent and solution preparation should be consistent with GB/T 601 and GB/T 603 Provisions. 4.1 Sensory test Take a proper amount of sample in a clean, dry white porcelain dish and observe its color and form under natural light. 4.2 Identification According to "vitamin A palmitate content determination" (4.3) under the test, the relative retention time of the main peak of the sample solution (4.3.4) should be consistent with the standard Solution (4.3.5) Vitamin A palmitate peak retention time consistent. 4.3 Vitamin A palmitate content determination Warning. The test should be carried out in dark conditions 4.3.1 Principle Samples with bromelain enzymatic hydrolysis may exist gelatin coating, then extracted with isopropanol vitamin A palmitate, liquid chromatography Determination, external standard method. 4.3.2 Reagents and solutions 4.3.2.1 Bromelain ( >.2000 GDU/g). 4.3.2.2 isopropanol (chromatographic purity). 4.3.2.3 Methanol (chromatographic purity). 4.3.2.4 Vitamin A alcohol reference substance (content ≥ 3150000IU/g). 4.3.2.5 Vitamin A acetate reference substance (content ≥ 2800000IU/g). 4.3.2.6 Vitamin A palmitate reference substance (content ≥ 1700000IU/g). 4.3.3 Instruments and Equipment 4.3.3.1 High Performance Liquid Chromatograph with UV detector or diode array detector. 4.3.3.2 electric oven temperature. 4.3.3.3 ultrasonic cleaner. 4.3.3.4 Analysis of balance. Sense of 0.1mg. 4.3.4 Preparation of sample solution Weigh the sample amount (about the equivalent of vitamin A palmitate 50000IU), accurate to 0.1mg, placed in 250mL brown volumetric flask , Add Bromelain (4.3.2.1) 20mg ~ 30mg, water 10mL, at 60 ℃ ~ 65 ℃ water bath ultrasonic 5min, remove the cold water But to room temperature, diluted with isopropyl alcohol (4.3.2.2) to the mark, shake. 4.3.5 standard solution preparation Weigh vitamin A palmitate reference substance (4.3.2.6) 0.05g, accurate to 0.1mg, placed in 50mL brown volumetric flask, add different Propanol (4.3.2.2) diluted to the mark, shake. 4.3.6 Reference chromatographic conditions Reference chromatographic conditions are as follows. --- Column. C18 column, column length 150mm, diameter 4.6mm, particle size 5μm or quite performance; --- Column temperature .35 ℃; --- Mobile phase. Methanol (4.3.2.3); --- Flow rate .1.5mL/min; --- Detection wavelength .325nm; --- Injection volume .20μL. 4.3.7 Determination steps Take the standard solution (4.3.5) and sample solution (4.3.4) respectively, filtered through 0.45μm membrane, injection analysis, record the chromatograms (vitamins A palmitate liquid chromatogram see Appendix A), according to external standard method to peak area calculation. 4.3.8 Calculation and representation of results 4.3.8.1 Vitamin A palmitate content The content of vitamin A palmitate X1, expressed in IU/g (IU/g), is calculated according to equation (1). X1 = A2 × m1 × 250 × C1 A1 × m2 × 500 (1) In the formula. A1 --- standard solution of vitamin A palmitate peak area; A2 --- sample solution of vitamin A palmitate peak area; m1 --- vitamin A palmitate quality of the reference substance, in grams (g); m2 --- the quality of the sample, in grams (g); 250 --- sample dilution volume, in milliliters (mL); 500 --- Vitamin A palmitate reference standard dilution volume, in milliliters (mL); C1 --- Vitamin A palmitate reference substance content in units of International Units per gram (IU/g). Take the arithmetic mean of two parallel determination results as the determination result, the result is retained to one decimal place. The absolute difference between two parallel determinations shall not be greater than 4.0% of the arithmetic mean of these two determinations. 4.3.8.2 Vitamin A palmitate content (in marked amount) Vitamin A palmitate content X2 (accounting for the amount), expressed in%, according to equation (2) calculation. X2 = X1 X × 100 (2) X1 --- Vitamin A palmitate content in units of International Units per gram (IU/g); X --- Vitamin A palmitate labeled amount, in units of international units per gram (IU/g). The result of the calculation is one digit after the decimal point. 4.4 Vitamin A alcohol and vitamin A acetate total content determination Warning. The test should be carried out in dark conditions 4.4.1 Principle Samples of vitamin A alcohol and vitamin A acetate by bromelain enzymatic hydrolysis, with isopropyl alcohol extraction, liquid chromatography analysis, external standard Legal quantity. 4.4.2 Preparation of standard solution 4.4.2.1 Vitamin A alcohol and vitamin A acetate stock solution Weigh about vitamin A alcohol reference substance (4.3.2.4) and vitamin A acetate reference substance (4.3.2.5) of about 0.02g (accurate to 0.01mg) In a 100mL brown volumetric flask, dilute to the mark with isopropanol (4.3.2.2) and shake well. Pro use now with. 4.4.2.2 Vitamin A alcohol and vitamin A acetate standard solution Draw vitamin A alcohol and vitamin A acetate stock solution each 1.00mL in the same 100mL brown volumetric flask with isopropanol (4.3.2.2) diluted to the mark, shake well, that is, too. 4.4.3 Preparation of sample solution With the determination of vitamin A palmitate content of the sample solution (4.3.4). 4.4.4 Determination Take the sample solution (4.4.3) and standard solution (4.4.2.2), 0.45μm filter membrane, according to the reference chromatographic conditions (4.3.6) injection analysis, Record the chromatograms (see Appendix A for the liquid chromatogram of retinol and vitamin A acetate). According to the standard solution peak retention Time qualitative, peak order followed by vitamin A alcohol and vitamin A acetate, peak area corresponding to the peak value of the peak, external standard method Its content. 4.4.5 Calculation and representation of results 4.4.5.1 Vitamin A alcohol and vitamin A acetate total content The total content of vitamin A and vitamin A acetate X3, expressed in IU/g, is calculated according to equation (3). X3 = A4 × m3 × 250 × C2 A3 × m2 × 10000 A6 × m4 × 250 × C3 A5 × m2 × 10000 (3) In the formula. A3 --- standard solution of vitamin A alcohol peak area; A4 --- sample solution of vitamin A alcohol peak area; m2 --- the quality of the sample, in grams (g); m3 --- Vitamin A alcohol reference substance quality, in grams (g); 250 --- sample dilution volume, in milliliters (mL); 10000 --- vitamin A alcohol and vitamin A acetate reference standard dilution volume, in milliliters (mL); C2 --- vitamin A alcohol reference substance content in units of International Units per gram (IU/g); A5 --- standard solution of vitamin A acetate peak area; A6 --- sample solution of vitamin A acetate peak area; m4 --- vitamin A acetate reference substance quality, in grams (g); C3 --- Vitamin A acetate reference substance content in units of International Units per gram (IU/g). Take the arithmetic mean of two parallel determination results as the determination result, the result is retained to one decimal place. The absolute difference between two parallel determinations shall not be greater than 30% of the arithmetic mean of the two determinations. 4.4.5.2 Vitamin A alcohol and vitamin A acetate total content (in marked amount) Vitamin A palmitate content X4 (accounting for the amount), expressed in%, according to equation (4) calculation. X4 = X3 X × 100 (4) X3 --- total content of Vitamin A and Vitamin A acetate in IU/g; X --- Vitamin A palmitate labeled amount, in units of international units per gram (IU/g). The result of the calculation is one digit after the decimal point. 4.5 granularity Particle size according to GB/T 5917.1 provisions of the method implementation. 4.6 Loss on drying Loss on drying according to the method specified in GB/T 6435. 4.7 heavy metals 4.7.1 Reagents and solutions 4.7.1.1 Sulfuric acid. Note that sulfuric acid is a strong corrosive liquid, the operator should wear safety goggles and gloves to prevent burns. 4.7.1.2 Nitric acid. 4.7.1.3 Hydrochloric acid. 4.7.1.4 Glycerin. 4.7.1.5 Lead standard solution .1000μg/mL. 4.7.1.6 Sodium hydroxide solution .40g/L. Note that sodium hydroxide is a strong corrosive liquid, the operator should wear safety goggles and gloves to prevent burns. 4.7.1.7 Ammonia solution (10%) Prepared according to GB/T 603 4.7.1.8 hydrochloric acid solution I. Take hydrochloric acid 63mL, add water to 100mL, shake. 4.7.1.9 hydrochloric acid solution II. Take hydrochloric acid 18mL, add water to 100mL, shake. 4.7.1.10 thioacetamide solution Take thioacetamide 4g, dissolved in water and diluted to 100mL, stored in a refrigerator. Before use Take 1.0 mL and the mixed solution [consisting of 15 mL of sodium hydroxide solution (4.7.1.6), 5.0 mL of water and glycerol (4.7.1.4)], 5.0 mL, water bath On the heating 20s, mix, cool, and immediately use. 4.7.1.11 Acetate buffer (pH3.5) Take 25g of ammonium acetate and add 25mL of water to dissolve. Add 38mL of hydrochloric acid solution I (4.7.1.8) Acid solution Ⅱ (4.7.1.9) or ammonia solution (4.7.1.7) Accurately adjust the pH to 3.5 (pH indicator), diluted with water to 100mL, shake. 4.7.1.12 phenolphthalein indicator solution. Prepared according to GB/T 603. 4.7.1.13 Preparation of lead standard working solution Pipette 2.00 mL of lead standard solution (4.7.1.5) into a.200 mL volumetric flask and dilute to volume with water Degree, shake (equivalent to 10μg of Pb per ml). 4.7.2 Preparation of sample solution Weigh the sample 1g (accurate to 0.01g), home porcelain crucible, slowly burning to fully carbonized, let cool. Add sulfuric acid (4.7.1.1) 0.5mL ~ 1mL humid, low temperature heating to sulfuric acid vapor removed, the ignition at 550 ℃ completely ashed, let cool. Add nitric acid (4.7.1.2) 0.5mL, Steam dry until the nitrogen oxide vapor removed, let it cool. Add hydrochloric acid (4.7.1.3) 2.0mL, set water bath and add water after 15mL, dropping ammonia solution (4.7.1.7) to phenolphthalein indicator solution (4.7.1.12) was reddish, coupled with acetate buffer (4.7.1.11) 2.0mL, after the solution was dissolved slightly heat 's colorimetric tube, diluted with water into 25mL, as B tube. 4.7.3 Preparation of standard colorimetric solution Another preparation of sample solution reagents, home-made porcelain crucible evaporated, add acetate buffer (4.7.1.11) 2.0mL and water 15mL, micro After thermal dissolution, remove the Nessler colorimetric tube, add lead standard working solution (4.7.1.13) 1.00mL, and then diluted with water into 25mL, as a tube. 4.7.4 Determination and determination of results In A, B two were added thioacetamide solution (4.7.1.10) each 2.0mL, shake, place 2min, with the same white paper, from the top to Under the perspective of observation and comparison of the color of the tube and the tube, such as the color of the tube was not deeper than the tube, then judged to comply with the provisions. 4.8 Total arsenic 4.8.1 Reagents and solutions 4.8.1.1 Hydrochloric acid. 4.8.1.2 Magnesia. 4.8.1.3 arsenic-free zinc particles to pass through the No. 1 screen of arsenic-free zinc is appropriate, such as the use of zinc particles larger, the amount should be increased as appropriate, the reaction time is extended To 1h. 4.8.1.4 arsenic standard solution .1000μg/mL. 4.8.1.5 Magnesium nitrate solution .150 g/L. 4.8.1.6 hydrochloric acid solution Take hydrochloric acid 18mL, add water to make 100mL, shake. 4.8.1.7 Potassium iodide solution, 165 g/L. The solution should be used with the new. 4.8.1.8 Acidic stannous chloride solution Take stannous chloride 20g, add hydrochloric acid (4.8.1.1) to dissolve into 50mL, filtered, shake. Validity 3 months. 4.8.1.9 lead acetate solution Take lead acetate 10g, add freshly boiled cold water dissolved, acetic acid was added dropwise to make the solution clear, add freshly boiled cold water To 100mL, shake well. 4.8.1.10 arsenic standard working solution preparation Draw arsenic standard solution (4.8.1.4) 5.00mL set 100mL flask, diluted with water to the mark, Shake well, and then draw 2.00mL, set 100mL flask, diluted with water to the mark, shake (equivalent to 1μg per ml of As). 4.8.1.11 Mercury bromide test strip Prepared in accordance with GB/T 603 and stored in a brown mill jar. 4.8.1.12 lead acetate cotton Take cotton wool, immersed in a solution of lead acetate solution (4.8.1.9) and water, an equal volume of mixed solution, after soaking, Lek to excess Of the solution, and make it loose, dry at below 100 ℃, stored in a ground glass jar spare. 4.8.1.13 phenolphthalein indicator solution. Prepared according to GB/T 603. 4.8.2 Analysis steps 4.8.2.1 Preparation of sample arsenic spots Take the sample 1.0g (accurate to 0.01g) in a porcelain crucible, add magnesium nitrate solution (4.8.1.5) 10mL and magnesium oxide 1g, mix, soak 4h, evaporated to dryness in a low temperature or water bath, slowly ignited with a small flame until completely carbonized, let cool. Ignition at 550 ℃ completely ashed, add water 2mL Wet ash, add phenolphthalein indicator solution (4.8.1.13) 1 drop, such as red, hydrochloric acid solution (4.8.1.6) was added dropwise to the red fade, transferred to a conical flask, Washed with water 21mL porcelain crucible wash, wash solution into the conical flask, plus hydrochloric acid (4.8.1.1) 5mL, add potassium iodide solution (4.8.1.7) 5mL and acidic stannous chloride solution (4.8.1.8) 5 drops at room temperature for 10min, add no arsenic zinc tablets 2g, immediately put the top plane Mercury bromide test strips (4.8.1.11) and airways with lead acetate cotton (4.8.1.12) are capped on a conical flask and the conical flask is placed at 25 ° C ~ 40 ℃ water bath, the reaction 45min, remove the mercury bromide test strips, that is, too. 4.8.2.2 Preparation of standard arsenic spots Another preparation of samples of arsenic stain reagents, set the porcelain crucible with the sample in the same treatment, into the conical flask, add hydrochloric acid (4.8.1.1) 5mL and Water 21mL, then draw arsenic standard working solution (4.8.1.10) 2.00mL, according to "sample arsenic spot preparation" (4.8.2.1) under the "add potassium iodide Liquid "from the same operation. 4.8.2.3 result judgment Mercury bromide test strips were removed and the color of the arsenic spot was compared with the naked eye. If the color of the arsenic spot of the sample was not deeper than the standard arsenic color, it was judged as conforming to the provisions.

5 inspection rules

5.1 sampling method According to GB/T 14699.1. 5.2 group approved With the same material, the same production process, produced in a row or continuous production of a uniform product as a production batch. 5.3 factory inspection The items listed in Chapter 3, Appearance and Traits, Vitamin A Palmitate, Vitamin A Alcohol and Vitamin A Acetate Total, Particle size, weight loss for the factory inspection items. 5.4 type test Type inspection items for all the requirements of Chapter 3. Product normal production, at least once every six months type test, but the following conditions One of the conditions should also be type tested. a) when the product is shaped b) there is a big change i......
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