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This standard replaces GB 15044-2009 Food additive - Carrageenan
The following main changes have been made with respect to GB 15044-2009:
——the index requirements and test methods for acid insolubles, pH, residual solvent (isopropanol and methanol), total bacterial count and escherichia coli are added;
——the index requirement for coliform bacteria is deleted;
——the test methods for sulfate (calculated by SO4), total ash and acid-insoluble ash are modified;
——the normative references for some test methods are adjusted to the latest versions.
National food safety standard
Food additive - Carrageenan
1 Scope
This standard is applicable to the food additive carrageenan which is obtained from Rhodophyceae plants by extraction and processing with water or alkali liquid. The product is a mixture of three basic types: K (Kappa), I (Iota) and λ (Lambda).
2 Technical requirements
2.1 Sensory requirements
Sensory requirements shall meet those specified in Table 1.
Table 1 Sensory requirements
Item Requirement Test method
Color and luster Off-white or pale yellow to pale brown Take a proper amount of specimen and put it into a clean and dry white porcelain dish, and observe its color and luster as well as state in natural light
State Powder or particles
2.2 Physical and chemical indexes
Physical and chemical indexes shall meet those specified in Table 2.
Table 2 Physical and chemical indexes
Item Index Test method
Sulphate (calculated by SO4), w/% 15~40 Annex A, A.3
Viscosity/ Pa·s ≥ 0.005 Annex A, A.4
Loss on drying, w/% ≤ 12.0 Direct drying methoda in GB 5009.3
Total ash, w/% 15~40 Annex A, A.5
Acid-insoluble ash, w/% ≤ 1 Annex A, A.6
Acid insolubles, w/% ≤ 15 Annex A, A.7
pH 8~11 Annex A, A.8
Residual solventb (isopropanol and methanol), w/% ≤ 0.1 Annex A, A.9
Plumbum (Pb)/ (mg/kg) ≤ 5.0 GB 5009.75 or GB 5009.12
Arsenic (As)/ (mg/kg) ≤ 3.0 GB 5009.76
Cadmium (Cd)/ (mg/kg) ≤ 2.0 GB 5009.15
Mercury (Hg)/ mg/kg ≤ 1.0 GB 5009.17
a Drying temperature: 105 ℃; duration: 4 h.
b It is only applicable to product with isopropanol or methanol as extraction solvent.
Note 1: Commercial carrageenan products shall be made from carrageenan which meets the requirements specified in this standard. Besides, it may contain sugars for standardization purposes, salts for special gelation or thickening effects, such as potassium chloride (sodium, calcium), sodium citrate, sodium hexametaphosphate and calcium lactate, as well as thickeners and emulsifiers brought in during the drying process.
Note 2: Ethanol, isopropanol and (or) methanol shall be used as the extraction solvent.
2.3 Microbial indexes
Microbial indexes shall meet those specified in Table 3.
Table 3 Microbial indexes
Item Index Test methoda
Total bacterial count/ (CFU/g) ≤ 5,000 GB 4789.2
Escherichia coli CFU/g ＜ 10 GB 4789.38
MPN/g ＜ 3.0
Salmonella (25 g) It shall not be detected GB 4789.4
a Under aseptic conditions, weigh 1.0g of specimen and dissolve it in 100 mL of phosphate buffer or normal saline to prepare a solution with a dilution of 1:100.
Annex A
Test method
A.1 General requirements
Unless otherwise specified, analytically pure reagents and Grade 3 water specified in GB/T 6682 are adopted for the purposes of this standard. Unless otherwise specified, the standard solution, the standard solution for impurity determination, preparations and products used in test are prepared according to GB/T 601, GB/T 602 and GB/T 603. The solution used in the tests refers to the aqueous solution if it is not indicated which solvent is used.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Ethanol solution: 85+15.
A.2.1.2 Potassium chloride solution: dissolve 2.5 g of potassium chloride in 100 mL of water.
A.2.1.3 Methylene blue solution: dissolve 1 g of methylene blue in 100 mL of water.
A.2.2 Analytical procedures
A.2.2.1 Weigh 4 g of specimen, add 200 mL of water, heat to about 80 ℃ and stir continuously until the specimen is completely dissolved. Replenish the moisture lost by evaporation with water, and cool the solution to room temperature, after which, the solution becomes a translucent viscous liquid and can produce gel-like matters.
A.2.2.2 Take 50 mL of the solution specified in A.2.2.1, add 200 mL of potassium chloride solution, reheat and mix it well, then take it out for cooling; stir the solution with a glass rod, if it turns to brittle colloid, it is the carrageenan which is mainly type Κ; if it turns to soft (elastic) colloid, it is the carrageenan which is mainly type I; if the solution does not turn into colloid, it is the carrageenan which is mainly type λ.
A.2.2.3 Take 5 mL of the solution specified in A.2.2.1 and add 1 drop of methylene blue solution, after which, it produces fibrous precipitation.
A.2.2.4 Determine the infrared absorption spectrum of the gel and non-gel components of the specimen prepared by the following method.
Weigh 2 g of specimen, add 200 mL of potassium chloride solution, stir for 1h and keep it still overnight. Then stir it for 1 h again and transfer it to the centrifuge tube (if the specimen diffusion solution is so sticky that can not be transferred, it may be diluted with no more than 200 mL of potassium chloride solution), and centrifuge the specimen for 15 min at a speed close to 1,000 r/min.
Remove the supernatant, add 200 mL of potassium chloride solution to the residue, stir and centrifuge again. Combine the supernatant obtained from the last two procedures, add ethanol solution with the volume equivalent to twice the volume of the supernatant to make it coagulate (retain the precipitate for later use), and recover the coagulum and wash it with 250 mL of ethanol solution. Squeeze the excess liquid from the coagulum and dry it at 60 °C for 2 h to obtain a non-gel component (carrageenan of type λ).
Foreword i
1 Scope
2 Technical requirements
Annex A Test method
