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GB 1886.239-2016 English PDF

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GB 1886.239-2016: National Food Safety Standard -- Food Additives -- Agar
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Basic data

Standard ID GB 1886.239-2016 (GB1886.239-2016)
Description (Translated English) National Food Safety Standard -- Food Additives -- Agar
Sector / Industry National Standard
Classification of Chinese Standard X41
Word Count Estimation 12,118
Date of Issue 2016-08-31
Date of Implementation 2017-01-01
Older Standard (superseded by this standard) GB 1975-2010
Regulation (derived from) Announcement of the State Administration of Public Health and Family Planning 2016 No.11
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.239-2016: National Food Safety Standard -- Food Additives -- Agar

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(Food safety national standard - Food additive - Agar) National Standards of People's Republic of China GB 1886.242-2016 National Food Safety Standard Food Additives ammonium glycyrrhizinate Issued on. 2016-08-31 2017-01-01 implementation People's Republic of China National Health and Family Planning Commission released GB 1886.242-2016 National Food Safety Standard Food Additives ammonium glycyrrhizinate

1 Scope

This standard applies to raw licorice (legume licorice GlycyrrhizauralensisFisch., Glycyrrhiza inflata Glycyrrhizain- flataBat. and Glycyrrhiza glabra GlycyrrhizaglabraL.), mentioned by the flooding, sulfuric acid (or hydrochloric acid) acidified precipitation, ethanol extraction, amide, knot Crystal and other processes to prepare food additive ammonium glycyrrhizinate. 2 chemical name, structural formula, molecular formula, relative molecular mass 2.1 Chemical Name Ammonium glycyrrhizinate 2.2 formula Formula 2.3 C42H61O16NH4 2.4 relative molecular mass 839.96 (according to 2007 international relative atomic mass)

3 Technical requirements

3.1 Sensory requirements Sensory requirements shall comply with the requirements of Table 1. GB 1886.242-2016 Table 1 Sensory requirements Project requires test methods Color white, yellowish-white or pale yellow Status powdery fine particles Take the right amount of sample is placed in a clean, dry white porcelain plate , Under natural light, observe its color and status 3.2 Physical and Chemical Indicators Physical and chemical indicators should be consistent with the provisions of Table 2. Table 2. Physical and chemical indicators Item Index Test Method Licorice ammonium content (18β- licorice ammonium meter, dry basis), w /% ≥ 65.0 Appendix A A.4 Loss on drying, w /% ≤ 7.0 Appendix A A.3 Specific rotation [α] 20 ° D/[(°) · mL · dm-1 · g-1] 45 ~ 53 in Appendix A A.5 Ash, w /% ≤ 0.5 A.6 in Appendix A Lead (Pb)/(mg/kg) ≤ 2.0 Appendix A A.7 Total arsenic (As)/(mg/kg) ≤ 2.0 Appendix A A.8 GB 1886.242-2016

Appendix A

Testing method A.1 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to the three water analytical reagent and GB/T 6682 regulations. test Test used in the standard solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T 602, GB/T 603 provisions prepared. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution. A.2 Identification Test A.2.1 Method summary After the case of alkali salts to produce ammonia, with ammonia and volatile basic characteristics of the top tube to make moist pH paper was a basic color, Kam The presence of other salts. A.2.2 Reagents and materials A.2.2.1 sodium hydroxide solution. 40g/L. A.2.2.2 pH test paper. A.2.3 Identification method Take a sample of about 0.2g ammonium licorice in 10mL tube, add about 1mL sodium hydroxide solution (A.2.2.1), shaking, quickly has Water wet pH paper into the mouth of the tube, to produce ammonia and volatile wet pH paper was to make a basic color. Note. If the solution is heated, the color reaction is more obvious. A.3 Determination of loss on drying A.3.1 Instruments and Equipment A.3.1.1 vacuum drying oven. A.3.1.2 weighing bottle. A.3.1.3 dryer. A.3.2 Procedure The weighing bottle placed in a vacuum oven, 78 ℃ ± 0.5 ℃, dried under 20mm Hg 30min, taken out into the dryer The cooled to room temperature, and weighed. Weigh 1g sample, accurate to 0.0001g, stoppered and weighed. Gently shake the horizontal lateral weighing bottle, Uniform distribution layer as a sample, is less than 5mm. The paved specimen weighing bottle placed in a vacuum oven, open the cork, in At 78 ℃ ± 0.5 ℃, 20mmHg conditions, drying under reduced pressure 6h, out into a dryer, stoppered, allowed to cool to room temperature, and weighed. A.3.3 Calculation Results Loss on drying mass fraction w1, according to equation (A.1) Calculated. GB 1886.242-2016 w1 = m1-m2 m × 100% (A.1) Where. m1 --- vacuum dried weighing bottle before adding the sample mass, in grams (g); m2 --- dried under reduced pressure weighing bottle plus sample mass, in grams (g); Numerical m --- sample mass, in grams (g). The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given absolute difference is not more than 1.0%. A.4 Determination of licorice ammonium content (18β- licorice ammonium meter, dry basis) of A.4.1 Method summary The sample was acetonitrile - water dissolved, filtered, measured by liquid chromatography (UV detector), external standard. When the calculation results, the sample Weigh the sample by subtracting the mass of the sample water quality, the result is a dry basis (C42H65NO16) Total mass fraction of ammonium glycyrrhizinate. A.4.2 Reagents and materials A.4.2.1 acetonitrile. HPLC grade. A.4.2.2 glacial acetic acid. pure class distinctions. A.4.2.3 0.45μm membrane (organic phase). A.4.2.4 licorice ammonium Standard. Purity ≥90% (HPLC or logo). Note 1. The licorice ammonium standard method used was ammonium licorice 18β- single component standard. Note 2. The standard non-aqueous titration (NT) or other non-HPLC method for the determination of identity, its content can not be directly used to calculate the value of liquid chromatography content. A.4.2.5 acetonitrile - water. acetonitrile and water mixed in equal volumes. A.4.2.6 acetonitrile - acetic acid - water. glacial acetic acid aqueous acetonitrile (38 161), mix and filter through 0.45μm (organic phase) is too Filter, fully degassed. A.4.3 Instruments A.4.3.1 performance liquid chromatography with UV detection. A.4.3.2 balance, a sense of the amount of 0.01mg. A.4.3.3 vacuum drying oven. A.4.4 Analysis step A.4.4.1 Standard Solution Weigh 12.5mg licorice ammonium standard, accurate to 0.01mg, placed in 25mL volumetric flask with acetonitrile - water (A.4.2.5) solution Solution, and to volume. Through 0.45μm membrane (organic phase) and filtered. Using now. A.4.4.2 Preparation of sample solution Weigh 50.0mg licorice ammonium samples, accurate to 0.01mg, placed in 100mL flask with acetonitrile - water (A.4.2.5) solution Solution to the mark by 0.45μm membrane (organic phase) filter, tested. A.4.4.3 reference chromatographic conditions A.4.4.3.1 Column. C18 column, length 150mm, internal diameter 4.6mm, particle size 5μm. Or equivalent separation column. A.4.4.3.2 mobile phase. acetonitrile - glacial acetic acid - water (A.4.2.6). A.4.4.3.3 flow rate. 1.0mL/min. A.4.4.3.4 column temperature. room temperature. GB 1886.242-2016 A.4.4.3.5 Injection volume. 10μL. A.4.4.4 Determination Followed by injection of licorice ammonium standard solution and sample solution was measured at a wavelength of 254nm at the external standard. Licorice ammonium HPLC Chromatograms and retention time, see Appendix B. A.4.5 Calculation Results Licorice ammonium content (18β- licorice ammonium meter, dry basis) of the mass fraction w2, according to equation (A.2) Calculated. w2 = V × cs × A m3 × (1-w1) × As × 100% (A.2) Where. V --- volume of the sample volume, in milliliters (mL); cs --- licorice ammonium standard solution concentration, in milligrams per milliliter (mg/mL); A --- sample solution chromatogram peak area licorice ammonium; Numerical m3 --- sample mass, in milligrams (mg); w1 --- Loss on drying of the sample mass fraction,%; As --- standard solution chromatogram peak area licorice ammonium. The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions Given absolute difference, not more than 5% of the arithmetic mean. A.5 Determination of specific rotation A.5.1 Reagents and materials A.5.1.1 ethanol. A.5.1.2 40% Ethanol - Aqueous Solution. Take 2 parts of ethanol and 3 parts of water are mixed. A.5.2 Instruments and Equipment Optical photometer, measure the minimum scale value 0.05 °. A.5.3 Analysis step A.5.3.1 Preparation of sample solution Weigh 1.5g (accurate to 0.01g) sample is not dried, and dissolved in 100mL of ethanol - water (A.5.1.2), and tested. A.5.3.2 Instrument Conditions A.5.3.2.1 measurement wavelength. sodium lamp D-line (589.3nm). A.5.3.2.2 measuring temperature. 20 ℃ ± 0.5 ℃. A.5.3.3 Determination Boot the instrument is stable, with ethanol - water (A.5.1.2) as a blank solution, zero calibration of the instrument (not auto-zero instrumentation required Determination of the blank value solution, deduction blank), the test solution filled with clean, dry optical tube, carefully remove air bubbles, tighten the lid after press Instrument Description Book operation, measured in a sample solution temperature 20 ℃ ± 0.5 ℃ condition, read optical values. L minus sign "-" indicates, D-positive No. "" means. GB 1886.242-2016 A.5.4 Calculation Results Specific rotation with [α] 20 ° D representation, numerical order "(°) · mL · dm-1 · g-1" meter, according to equation (A.3) calculations. [Α] 20 ° D = α × 100 l × (m4-m4 × w1) (A.3) Where. Optical rotation α --- sample solution measured in degrees (°); 100 --- sample was dissolved in ethanol ammonium licorice - the volume of the aqueous solution, in milliliters (mL); L --- optical tube length in decimeters (DM); m4 --- said the quality licorice ammonium sample in grams (g); w1 --- Loss on drying of the sample mass fraction,%. The arithmetic average of the three parallel determination results of the measurement results, reserved to the nearest whole number. A.6 Determination of ash A.6.1 Instruments and Equipment High temperature furnace. A.6.2 Analysis step Weigh 3g sample (accurate to 0.0001g), placed in 100mL constant weight porcelain crucible, Fo Tan of small to smoking. Move to 550 ℃ ± 25 ℃ High-temperature furnace burning, until the sample completely gray (about 3h), dryer cooled to room temperature, weighed, repeated ignition until constant weight (around twice called The difference between the amount of not more than 0.5mg). A.6.3 Calculation Results Ash mass fraction w3, according to equation (A.4) Calculated. w3 = m5-m6 m7 × 100% (A.4) Where. After m5 --- burning crucible plus ash mass, in grams (g); m6 --- crucible mass in grams (g); m7 --- sample mass, in grams (g). The results parallel arithmetic mean of the measurement results shall prevail (2 decimal places). In two independent test repeated conditions Given absolute difference is not more than 0.1%. A.7 Lead (Pb) Determination Lead content in the method according to GB 5009.12 determination, samples were dry ashing. A.8 Determination of total arsenic (As) of Arsenic at levels determined by the method in GB 5009.11. GB 1886.242-2016

Appendix B

Licorice ammonium liquid chromatogram and reference retention time of each component Licorice ammonium liquid chromatography is shown in Figure B.1, Figure B.2. Figure B.1 licorice ammonium standard (18β- licorice ammonium) liquid chromatograph Figure B.2 licorice ammonium sample liquid chromatogram

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