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GB 1886.361-2022 (GB1886.361-2022)

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GB 1886.361-2022: PDF in English

GB 1886.361-2022
National food safety standard - Food additive - Sodium
copper chlorophyllin
ISSUED ON. JUNE 30, 2022
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Molecular formula and relative molecular mass... 3
3 Technical requirements... 3
Annex A Inspection methods... 5
Annex B Microwave digestion temperature raise program... 12
Annex C Reference gas chromatogram of solvent residues in specimen solution... 13
National food safety standard - Food additive - Sodium
copper chlorophyllin
1 Scope
This document is applicable to sodium copper chlorophyllin, a food additive, that
chlorophyll is extracted from silkworm sand or grass (such as tall fescue, lucerne,
nettle), spirulina and other plants as raw materials, or directly uses chlorophyll as raw
material, and then is prepare by copper substitution reaction. The solvents used are
acetone, diazomethane, methanol, ethanol, isopropanol, n-hexane and (or) petroleum
ether (boiling range is 90°C~120°C).
2 Molecular formula and relative molecular mass
2.1 Molecular formula
Copper chlorophyllin a (C55H72CuN4O5)
Copper chlorophyllin b (C55H70CuN4O6)
2.2 Relative molecular mass
Copper chlorophyllin a. 932.75 (according to 2018 international relative atomic mass)
Copper chlorophyllin b. 946.73 (according to 2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall meet the requirements of Table 1.
3.2 Physical and chemical indicators
Physical and chemical indicators shall meet the requirements of Table 2.
Annex A
Inspection methods
A.1 General
Unless otherwise specified, the reagents and water used in this Standard refer to
analytically pure reagents and grade three water specified in GB/T 6682.The standard
solutions, standard solutions used for determination of impurities, preparations and
products shall be prepared in accordance with the provisions of GB/T 601, GB/T 602
and GB/T 603, unless other requirements are specified. The solution used in the test
refers to the aqueous solution when the solvent is not specified.
A.2 Identification test
A.2.1 Maximum absorption peak and absorbance ratio range
Take the specimen solution in A.3.3.1 Determination of chlorophyll content. There are
maximum absorption peaks in the two wavelength ranges of 405nm ± 3nm and 635nm
± 5nm. The absorbance ratio of the two measurements is between 3.2~4.0.
A.2.2 Copper ion test
A.2.2.1 Reagents and materials
A. Sulfuric acid.
A. Hydrochloric acid solution. 1+3.
A. Sodium diethyldithiocarbamate solution. 1g/L.
A.2.2.2 Analysis steps
Take 1g of specimen. Place in a crucible that has been burnt to constant weight at 800°C
± 25°C. Slowly heat until the specimen is completely carbonized. Cool the carbonized
specimen. Use 0.5mL~1mL of sulfuric acid to wet the residue. Continue to heat until
the sulfuric acid vapor escapes. Burn the residue to a heavy weight in a high temperature
furnace at 800°C ± 25°C. Add 10mL of hydrochloric acid solution to the residue. Heat
on the water bath to dissolve. After filtration, add water to 10mL. Take 5mL of the
above solution. Add 0.5mL of sodium diethyldithiocarbamate solution. Produce a
reddish-brown precipitate.
A.3 Determination of chlorophyll content
A.3.1 Reagents and materials
A.3.1.1 Anhydrous ether.
A.3.1.2 Disodium hydrogen phosphate solution (0.15mol/L). Weigh 53.7g of disodium
hydrogen phosphate (Na2HPO4 • 12H2O). Add water to dissolve. Dilute and set volume
to 1000mL.
A.3.1.3 Potassium dihydrogen phosphate solution (0.15mol/L). Weigh 20.4g of
potassium dihydrogen phosphate (KH2PO4). Add water to dissolve. Dilute and set
volume to 1000mL.
A.3.1.4 Phosphate buffer (pH 7.5). Measure disodium hydrogen phosphate solution
(0.15mol/L) and potassium dihydrogen phosphate solution (0.15mol/L) respectively.
Mix by volume ratio of 21.4.
A.3.1.5 Solution A. copper chloride-methanol solution (5%).
A.3.1.6 Solution B. sodium hydroxide-methanol solution (10%).
A.3.2 Instruments and equipment
A.3.2.1 Spectrophotometer.
A.3.2.2 Constant temperature water bath.
A.3.2.3 Separatory funnel (250mL).
A.3.3 Analysis steps
A.3.3.1 Preparation of specimen solution
Weigh 1g of specimen, to the nearest of 0.0002g. Place in an Erlenmeyer flask. Add
50mL~60mL of anhydrous ether to dissolve. Add 1mL of solution A. Heat to reflux for
15min in a constant temperature water bath at 50°C ± 2°C. Remove. Add 2mL of
solution B. Shake well. Continue to heat to reflux for 20min in a constant temperature
water bath at 50°C ± 2°C. Shake intermittently throughout the process. Make sure the
reaction is complete. After reaction, remove the Erlenmeyer flask. Cool. Add a little
water. Shake well. Transfer to a separatory funnel. Then use an appropriate amount of
water to wash the Erlenmeyer flask in several times. The washing liquid is transferred
to the separatory funnel. Shake well and let stand for at least 1h.
After the liquid in the separatory funnel is separated, filter the bottom liquid. Note that
the interfacial layer remains in the separatory funnel. Do not filter down to avoid
clogging filter paper. After filtration, rinse the upper acetyl layer and interface with
water until the washed water layer is colorless. The washing liquid is merged into the
lower filtrate. Discard the upper ether layer and interface. Use water to wash the filter
paper several times until almost it is almost colorless. The washing liquid is combined
into the lower filtrate. Keep all filtrates.
Transfer the filtrate to another separatory funnel. Use 40mL of anhydrous ether to shake
and wash. Place still for 15min. Transfer the lower liquid to a 250mL volumetric flask.
5mL of nitric acid. Digest the specimen according to the operation steps of microwave
digestion. Refer to B.1 for digestion conditions. Cool. Take out the digestion tank. Acid
to about 1mL at 120°C~140°C. After the digestion tank is cooled, transfer the digest to
a 25mL volumetric flask. Use a small amount of grade two water to wash the digestion
tank 2~3 times. Combine washing solution in the volumetric flask. Use grade two water
to set volume to the scale. Mix well for future use. At the same time, conduct reagent
blank test.
A.4.3.2 Dry ashing
Weigh 0.1g of specimen, to the nearest of 0.0002g. Heat in a crucible over low heat.
Carbonize to it is smokeless. Transfer to a 550°C muffle furnace. Conduct ashing for
3h~4h. Cool and take it out. For incompletely-ashed specimens, add several drops of
nitric acid. Heat with small fire. Steam dry carefully. Then transfer to the 550°C muffle
furnace. Continue ashing 1h~2h till the specimen is white grey. Cool and take out. Use
an appropriate amount of nitric acid solution (1+1) to dissolve. Use water to set volume
to 10mL. Mix well for future use. At the same time, conduct the blank test.
A.4.4 Analysis steps
Except for the specimen processing, other steps are determined according to the
methods specified in GB 5009.13.
A.5 Determination of free copper (Cu)
A.5.1 Reagents and materials
Same with GB 5009.13.
A.5.2 Instruments and equipment
Same with GB 5009.13.
A.5.3 Specimen processing
Weigh 0.1g of specimen, to the nearest of 0.0002g. Place in an Erlenmeyer flask. Add
20mL of anhydrous ether to dissolve. Then add 100mL of water. Cover with the stopper.
Shake 1min. Transfer to a 125mL separatory funnel. Place still for 30min. Use double-
layer filter paper to filter the lower liquid in the separatory funnel. If the filtrate is
colored, filter again with double-layer filter paper until the filtrate is colorless. The
filtrate shall be the specimen solution.
A.5.4 Analysis steps
Except for the specimen processing, other steps are determined according to the
methods specified in GB 5009.13.
A.6 Determination of solvent residues (dichloromethane, methanol, isopropanol,
n-hexane, n-heptane)
A.6.1 Reagents and materials
A.6.1.1 Water. Grade one water specified in GB/T 6682.
A.6.1.2 Standard product of test component. Dichloromethane, methanol, isopropanol,
n-hexane, n-heptane. Chromatographically pure.
A.6.1.3 Internal standard product. 3-methyl-2-pentanone. Chromatographically pure.
A.6.1.4 N-methylpyrrolidone.
A.6.2 Instruments and equipment
Gas chromatograph. Equipped with hydrogen flame ionization detector (FID) and
headspace specimen injector.
A.6.3 Reference chromatographic conditions
A.6.3.1 Chromatographic column. Quartz capillary column (Φ 0.53mm×30m). Coating
is dimethyl polysiloxane. Thickness is 5µm. Or chromatographic columns with
equivalent performance.
A.6.3.2 Carrier gas. Nitrogen.
A.6.3.3 Carrier gas flow rate. 5 mL/min.
A.6.3.4 Column temperature. Maintain at 35°C for 5min. Raise to 90°C at 5°C/min.
Maintain for 6min.
A.6.3.5 Inlet temperature. 140°C.
A.6.3.6 Detector temperature. 300°C.
A.6.3.7 Injection volume. 1.0mL.
A.6.4 Reference headspace injection conditions
A.6.4.1 Specimen heating temperature. 60°C.
A.6.4.2 Specimen heating time. 10min.
A.6.4.3 Syringe temperature. 90°C.
A.6.4.4 Mass transfer temperature. 100°C.
A.6.5 Analysis steps
A.6.5.1 Preparation of internal standard solution
(Above excerpt was released on 2022-08-21, modified on 2022-08-21, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GB1886.361-2022