GB 8817-2001 English PDF

GB 8817-2001: Food additive Caramel (Sulfite ammonia caramel, ammonia caramel, plain caramel)
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GB 8817-2001
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.220.20
X 41
Replacing GB 8817-1998
Food additive - Caramel (Sulfite ammonia caramel,
ammonia caramel, plain caramel)
ISSUED ON: AUGUST 06, 2001
IMPLEMENTED ON: FEBRUARY 01, 2002
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Requirements ... 4
4 Test method ... 5
5 Inspection rules ... 11
6 Marking, packaging, transportation, storage ... 11
Food additive - Caramel (Sulfite ammonia caramel,
ammonia caramel, plain caramel)
1 Scope
This standard specifies the technical requirements, test methods, inspection rules,
packaging, marking, storage, transportation requirements for liquid and powdered
caramel made by ammonium sulfite method, ammonia method, plain method.
This standard applies to liquid and powdered caramel made by ammonium sulfite
method, ammonia method, plain method, using sucrose, starch syrup, xylose mother
liquor, etc. as raw materials. It is used as colorants in food.
2 Normative references
The provisions contained in the following standards constitute the provisions of this
standard through reference in this standard. When this standard was published, the
versions shown were all valid. All standards are subject to revision. Parties using this
standard should explore the possibility of using the latest version of the following
standards.
GB/T 602-1988 Chemical reagent - Preparations of stock standard solutions
GB/T 5009.5-1985 Method for determination of protein in foods
GB/T 5009.17-1996 Method for determination of total mercury in foods
GB/T 5009.34-1996 Method for determination of sulfite in foods
GB/T 8449-1987 Method for determination of lead in food additives
GB/T 8450-1987 Method for determination of arsenic in food additives
GB/T 8451-1987 Method for limit test of heavy metals in food additives
3 Requirements
3.1 Sensory indicators
3.1.1 Color and appearance: Dark brown, thick liquid or powdery.
4.2 Determination of absorbance
Weigh 0.5 g of sample (accurate to 0.002 g). Use water to make the volume reach to the
mark in a 500 mL volumetric flask; use a 1 cm cuvette to measure its absorbance at 610
nm with a spectrophotometer.
4.3 Determination of loss on drying
4.3.1 Determination method
Weigh 2 g of sample (accurate to 0.0002 g) in a weighing bottle that has been weighed
constant. Dry at 105 °C for 2 h. Cool it. Weigh it.
4.3.2 Expression of analysis results
Where:
X1 - Loss on drying, %;
m1 - Mass of weighing bottle and sample before drying, g;
m2 - Mass of weighing bottle and sample after drying, g;
m - Mass of sample, g.
4.4 Determination of ammonia nitrogen
4.4.1 Reagents and solutions
4.4.1.1 Boric acid (GB/T 628): 2% solution.
4.4.1.2 Methyl red-bromocresol green mixed indicator solution: Mix 5 parts of 0.2%
bromocresol green ethanol solution and 1 part of 0.2% methyl red ethanol solution.
4.4.1.3 Magnesium oxide (HGB 1294).
4.4.1.4 Hydrochloric acid (GB/T 622): 0.1 mol/L solution, which is prepared and
calibrated according to GB/T 602.
4.4.2 Determination method
Weigh 5g of sample (accurate to 0.01 g). Place it in a 500 mL distillation flask. Add 2
g of magnesium oxide and 200 mL of water. Distill by direct fire. The distillate is
absorbed in 5 mL of 2% boric acid solution with 5 drops of mixed indicator solution.
When the distillate reaches about 100 mL, stop distillation and titrate the distillate with
0.1 mol/L hydrochloric acid, until it turns gray-red.
A and B are mixed in equal amounts before use.
4.6.1.9 4-Methylimidazole standard solution
Weigh the sample 4-methylimidazole (accurate to 0.1000 g). Place it in a 100 mL
volumetric flask. Add 95% ethanol to the mark. Each 1 mL of this solution is equivalent
to 1.0 mg of 4-methylimidazole.
Before use, use 95% ethanol to dilute it, to the level that each 1 mL is equivalent to 0.1
mg of 4-methylimidazole standard solution.
4.6.2 Method and steps
4.6.2.1 Extraction
Weigh 5 g of sample (accurate to 0.01 g). Add 15 mL of water to dissolve. Add 15 mL
of 10% sodium carbonate. Add 80 mL of chloroform-anhydrous ethanol mixed solution
to a 250 mL separatory funnel. Shake vigorously for 4 min ~ 5 min. After complete
layering, collect the chloroform-anhydrous ethanol extract in a 250 mL stoppered
conical flask. Use 70 mL of chloroform-anhydrous ethanol mixed solution to extract
the above water layer once. Combine the extracts. Add 20 mL of 0.05 mol/L sulfuric
acid to the extract. Shake vigorously 60 times. Separate the water layer. Concentrate
this solution to 2 mL ~ 3 mL in a 60 °C ~ 70 °C water bath. Slowly add about 0.2 g of
sodium bicarbonate fine powder, until no bubbles are generated. Use ethanol to dissolve
it to 5 mL.
4.6.2.2 Plate preparation
Weigh 3 g of silica gel (GF 254). Add 1 mL of 80% sodium bicarbonate solution and 6
mL of distilled water. Mix well and apply on a 125 mm×85 mm thin plate. Dry naturally
in the air. Put it in an oven at 120 °C for 2 minutes. After taking it out, put it in a dryer
for use.
4.6.2.3 Spotting
Spot 10 μL, 20 μL, 30 μL of 4-methylimidazole standard solution and 100 μL of sample
diluent on the thin plate, respectively.
Develop the thin plate in the developing agent until the solvent front reaches 10 cm.
Take out the thin plate. Blow dry it. Spray it with a newly prepared color developer.
Within 5 min ~ 10 min, the yellow spot of 4-methylimidazole can reach the deepest
depth and remain stable for several hours. According to the size and color depth of the
spot compared with the standard spot, determine the content of 4-methylimidazole in
the sample.
4.6.3 Expression of analysis results
Where:
X3 - 4-methylimidazole content, %;
c - Amount of sample spot equivalent to standard spot, µg;
m - Sample mass, g;
V1 - Spot volume, μL;
V2 - Total volume of sample solution, μL;
A610 - Absorbance of sample at 610 nm;
0.1/A610 - Content converted to chromaticity of 0.1.
4.7 Determination of arsenic
It is determined by arsenic spot method after wet digestion in accordance with GB/T
8450-1987.
4.8 Determination of lead
It is determined by wet digestion in accordance with GB/T 8449-1987.
4.9 Determination of heavy metals
It is determined by wet digestion in accordance with GB/T 8451-1987.
4.10 Determination of total nitrogen
It is determined according to GB/T 5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB 1294).
4.11.1.2 Magnesium nitrate [Mg(NO3)2·6H2O] (HG 3-1077).
4.11.1.3 Sucrose (HG 3-1001).
4.11.1.4 Nitric acid (GB/T 626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T 622).
5 Inspection rules
5.1 The same type of products with intact packaging produced by the same equipment
by the same shift are considered as a batch.
5.2 Randomly select samples from each batch of products. Select small samples of 5%
of the number of pieces or barrels of liquid products in each batch (at least 3 pieces or
3 barrels). Take not less than 500 mL of samples from each piece (or barrel), or 2 bags
for powder product (250 g sample from each bag). The sampled samples shall be mixed
quickly and evenly; respectively contained in two clean, dry large-mouth bottles,
labeled with the manufacturer's name, batch and sampling date. One copy shall be sent
to the laboratory for testing, whilst the other copy shall be kept for future reference.
5.3 Drying loss (solid) and absorbance are mandatory inspection items. Arsenic, lead,
heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen,
total sulfur are type spot inspection items.
5.4 If one of the indicators in the inspection does not meet this indicator, double the
number of products from the same batch shall be performed for re-inspection. If there
is still one item in the re-inspection result that does not meet this standard, the batch of
products shall be judged as unqualified.
5.5 If the supplier and the purchaser have objections to the product quality, the two
parties may negotiate and select the relevant statutory arbitration department to proceed,
in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging shall be firmly marked with the product name, manufacturer
name, address, trademark, model, standard number, production date, net content,
storage period, production license, batch number, etc. The words "food additives" shall
also be marked.
6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards shall
be used. The liquid specifications are 2, 10, 20, 30 kg; the powder specifications are 0.5,
1, 2.5, 10 kg, or packaged according to the specifications required by the buyer. The
sealing shall be tight; the liquid and powder are all packaged with corrugated paper.
6.3 Storage
The product shall be stacked in a ventilated, clean, dry place; it shall not be mixed with
GB 8817-2001
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.220.20
X 41
Replacing GB 8817-1998
Food additive - Caramel (Sulfite ammonia caramel,
ammonia caramel, plain caramel)
ISSUED ON: AUGUST 06, 2001
IMPLEMENTED ON: FEBRUARY 01, 2002
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Requirements ... 4
4 Test method ... 5
5 Inspection rules ... 11
6 Marking, packaging, transportation, storage ... 11
Food additive - Caramel (Sulfite ammonia caramel,
ammonia caramel, plain caramel)
1 Scope
This standard specifies the technical requirements, test methods, inspection rules,
packaging, marking, storage, transportation requirements for liquid and powdered
caramel made by ammonium sulfite method, ammonia method, plain method.
This standard applies to liquid and powdered caramel made by ammonium sulfite
method, ammonia method, plain method, using sucrose, starch syrup, xylose mother
liquor, etc. as raw materials. It is used as colorants in food.
2 Normative references
The provisions contained in the following standards constitute the provisions of this
standard through reference in this standard. When this standard was published, the
versions shown were all valid. All standards are subject to revision. Parties using this
standard should explore the possibility of using the latest version of the following
standards.
GB/T 602-1988 Chemical reagent - Preparations of stock standard solutions
GB/T 5009.5-1985 Method for determination of protein in foods
GB/T 5009.17-1996 Method for determination of total mercury in foods
GB/T 5009.34-1996 Method for determination of sulfite in foods
GB/T 8449-1987 Method for determination of lead in food additives
GB/T 8450-1987 Method for determination of arsenic in food additives
GB/T 8451-1987 Method for limit test of heavy metals in food additives
3 Requirements
3.1 Sensory indicators
3.1.1 Color and appearance: Dark brown, thick liquid or powdery.
4.2 Determination of absorbance
Weigh 0.5 g of sample (accurate to 0.002 g). Use water to make the volume reach to the
mark in a 500 mL volumetric flask; use a 1 cm cuvette to measure its absorbance at 610
nm with a spectrophotometer.
4.3 Determination of loss on drying
4.3.1 Determination method
Weigh 2 g of sample (accurate to 0.0002 g) in a weighing bottle that has been weighed
constant. Dry at 105 °C for 2 h. Cool it. Weigh it.
4.3.2 Expression of analysis results
Where:
X1 - Loss on drying, %;
m1 - Mass of weighing bottle and sample before drying, g;
m2 - Mass of weighing bottle and sample after drying, g;
m - Mass of sample, g.
4.4 Determination of ammonia nitrogen
4.4.1 Reagents and solutions
4.4.1.1 Boric acid (GB/T 628): 2% solution.
4.4.1.2 Methyl red-bromocresol green mixed indicator solution: Mix 5 parts of 0.2%
bromocresol green ethanol solution and 1 part of 0.2% methyl red ethanol solution.
4.4.1.3 Magnesium oxide (HGB 1294).
4.4.1.4 Hydrochloric acid (GB/T 622): 0.1 mol/L solution, which is prepared and
calibrated according to GB/T 602.
4.4.2 Determination method
Weigh 5g of sample (accurate to 0.01 g). Place it in a 500 mL distillation flask. Add 2
g of magnesium oxide and 200 mL of water. Distill by direct fire. The distillate is
absorbed in 5 mL of 2% boric acid solution with 5 drops of mixed indicator solution.
When the distillate reaches about 100 mL, stop distillation and titrate the distillate with
0.1 mol/L hydrochloric acid, until it turns gray-red.
A and B are mixed in equal amounts before use.
4.6.1.9 4-Methylimidazole standard solution
Weigh the sample 4-methylimidazole (accurate to 0.1000 g). Place it in a 100 mL
volumetric flask. Add 95% ethanol to the mark. Each 1 mL of this solution is equivalent
to 1.0 mg of 4-methylimidazole.
Before use, use 95% ethanol to dilute it, to the level that each 1 mL is equivalent to 0.1
mg of 4-methylimidazole standard solution.
4.6.2 Method and steps
4.6.2.1 Extraction
Weigh 5 g of sample (accurate to 0.01 g). Add 15 mL of water to dissolve. Add 15 mL
of 10% sodium carbonate. Add 80 mL of chloroform-anhydrous ethanol mixed solution
to a 250 mL separatory funnel. Shake vigorously for 4 min ~ 5 min. After complete
layering, collect the chloroform-anhydrous ethanol extract in a 250 mL stoppered
conical flask. Use 70 mL of chloroform-anhydrous ethanol mixed solution to extract
the above water layer once. Combine the extracts. Add 20 mL of 0.05 mol/L sulfuric
acid to the extract. Shake vigorously 60 times. Separate the water layer. Concentrate
this solution to 2 mL ~ 3 mL in a 60 °C ~ 70 °C water bath. Slowly add about 0.2 g of
sodium bicarbonate fine powder, until no bubbles are generated. Use ethanol to dissolve
it to 5 mL.
4.6...