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GB 28401—2012 Food Additives Phospholipids

national standards of People's Republic of China
GB 28401—2012
National food safety standards
Food additive
2012-05-17 Released 2012-07-17 Implementation
Ministry of Health and Welfare of the People's Republic of China
GB 28401—2012
National food safety standards
Food additive
1 Scope
This standard is applicable to food additive phospholipids prepared by the steps of dehydration, de-mixing, decolorization or degreasing, using vegetable oilseeds such as soybean and sunflower seeds or their processing by-products as the main raw materials.
2 Technical requirements
2.1 Sensory requirements: It should meet the requirements of Table 1.
Table 1 Sensory requirements
Project requirements test method
Color Yellow to brown Take an appropriate amount of sample in a clean transparent glass
The smell has the unique smell of phospholipids, no odor, in the dish, under natural light, observe its color
State viscous liquid, cream, powder or granules and state, and smell it
2.2 Physical and chemical indicators: should meet the requirements of Table 2.
Table 2 Physical and chemical indicators
Item indicator test method
Acetone insoluble matter, w/% ≥ 60 SN/T 0802.2 a
Dry reduction, w/% ≤ 2.0 GB 5009.3 Direct drying method b
N-hexane insoluble matter, w/% ≤ 0.3 Appendix A A.3
Acid value (in KOH) / (mg / g) ≤ 36 Appendix A A.4
Peroxide value / (meq / kg) ≤ 10 Appendix A A.5
Heavy metal (in Pb) / (mg / kg) ≤ 20 GB / T 5009.74
Total arsenic (as As) / (mg / kg) ≤ 3.0 GB/T 5009.11
Residual solvent / (mg / kg) ≤ 50 GB / T 5009.37 residual solvent
a In the calculation of the results, the "ether insoluble content" is replaced by the "n-hexane insoluble content". b Drying temperature and time are 105 °C and 1 h, respectively.
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GB 28401—2012
Appendix A
Testing method
A.1 General provisions
The reagents and water used in this standard refer to the analytical reagents and the tertiary water specified in GB/T 6682-2008 when no other requirements are specified. The standard titration solution used in the test, the standard solution for the determination of impurities, preparations and products shall be prepared according to the provisions of GB/T 601, GB/T 602 and GB/T 603 when no other requirements are specified. The solution used in the test refers to an aqueous solution when it is not indicated which solvent is used.
A.2 Identification test
A.2.1 Take 0.5 mL of 0.5% ethanol solution in a test tube, add 1-2 drops of 5% cadmium chloride ethanol solution to produce a white precipitate.
A.2.2 Take 10% ethanol solution of 2% sample in a test tube, add potassium citrate solution (take 8 g of lanthanum nitrate, add 20 mL of nitric acid to dissolve;
Take another 27.2 g of potassium iodide, add 50 mL of water to dissolve, combine the above two solutions, dilute to 100 mL with water and add 1 to 2 drops to produce brick red.
precipitation.
A.3 Determination of n-hexane insoluble matter
A.3.1 Reagents and materials
Hexane.
A.3.2 Instruments and equipment
A.3.2.1 Filter: 500 mL.
A.3.2.2 Glass sand core: G3.
A.3.3 Analysis steps
A.3.3.1 Dry the clean crucible to a constant weight in an oven at 101 °C ~ 105 °C.
A.3.3.2 Weigh 10.0 g of the sample with uniformity, accurate to 0.0001 g, place in a beaker, add about 100 mL of n-hexane, stir and dissolve with a glass rod, and then filter through a constant weight of hydrazine.
A.3.3.3 Wash the beaker and glass rod twice with 25 mL of n-hexane and transfer all the insoluble matter into the crucible. Wash the inner wall and insoluble matter with n-hexane, and finally remove the residual n-hexane from the crucible.
A.3.3.4 Remove the sputum and wipe the outer wall with a small amount of n-hexane. The crucible is dried in an oven at 101 ° C to 105 ° C for 1 h, taken out, placed in a desiccator, cooled to room temperature, and weighed. Dry for another 20 min, cool and weigh until constant weight.
A.3.4 Calculation of results
The content of n-hexane insolubles is expressed by mass fraction w1, and the value is expressed in %, calculated according to formula (A.1):
m  m
1
w 1 
In the formula:
2
m
 100 % „„„ „ „ „ „ „ „ „ „ „ „ „ „ „ „ „
M1 - the total mass of open and insoluble matter, in grams (g); m2 - the value of open mass, in grams (g);
m - the value of the sample mass in grams (g).
The experimental results are based on the arithmetic mean of the parallel determination results. The absolute difference between two independent determinations obtained under repeatability conditions shall not exceed 5% of the arithmetic mean.
A.4 Determination of acid value
A.4.1 Reagents and materials
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GB 28401—2012
A.4.1.1 petroleum ether.
A.4.1.2 Sodium hydroxide standard titration solution: c (NaOH) = 0.1 mol / L.
A.4.1.3 Neutral ethanol: The mass fraction is 95%. Before use, the phenolphthalein indicator solution was used as an indicator, and the solution was titrated with a sodium hydroxide standard titration solution until the solution was reddish, and the end point was maintained for 5 s without fading.
A.4.1.4 Phenolphthalein indicator solution: 10 g/L.
A.4.2 Analysis steps
Weigh approximately 2 g of the well-mixed sample to the nearest 0.001 g, place in a 250 mL Erlenmeyer flask, add 50 mL of petroleum ether, and gently shake
Dissolve, then add 50 mL of neutral ethanol and shake well. Add 4 drops of phenolphthalein indicator solution, quickly titrate with sodium hydroxide standard titration solution, while
When the drip edge is shaken, close to the end point, slow down the titration speed to 1~2 drops each time, until the pink appears and maintains 5 s without fading.
A.4.3 Calculation of results
The acid value is expressed in terms of mass fraction w2 of potassium hydroxide (KOH), and the value is expressed in milligrams per gram (mg/g), calculated according to formula (A.2):
w 2 
In the formula:
V  c  56 1
m 0
„„„„„„„„„„„„„„„„ (A.2)
V——the value of the volume of sodium hydroxide standard titration solution consumed by the titration, in milliliters (mL); c—the value of the concentration of sodium hydroxide standard titration solution, in moles per liter (mol/L);
56.1 - The molar mass of potassium hydroxide, in grams per mole (g/mol) [M(KOH) = 56.1]; m0 - the mass of the sample, in grams (g).
The experimental results are based on the arithmetic mean of the parallel determination results. The absolute difference between two independent determinations obtained under repeatability conditions shall not exceed 5% of the arithmetic mean.
A.5 Determination of peroxide value
A.5.1 Reagents and materials
A.5.1.1 Mixture of acetic acid and chloroform: Mix 3 parts of glacial acetic acid with 2 parts of chloroform in a volume ratio of 3:2.
A.5.1.2 Saturated potassium iodide solution: newly formulated and free of free iodine and iodate. Make sure that crystals are present in the solution and store in a dark place. If you add 0.5 mL of saturated potassium iodide solution and 2 drops of starch indicator solution to 30 mL of acetic acid and chloroform mixture, if the solution appears blue and requires more than 1 drop of sodium thiosulfate standard titration solution, you need to reconstitute this. Solution.
A.5.1.3 sodium thiosulfate standard titration solution: c (Na2S2O3) = 0.01 mol / L, the c (Na2S2O3) = 0.1 mol / L sodium thiosulfate standard titration solution diluted 10 times.
A.5.1.4 Starch indicator solution: 10 g / L.
Note: All reagents and water above must not contain dissolved oxygen.
A.5.2 Instruments and equipment
Laboratory routine instruments. All utensils used must not contain reducing or oxidizing substances. The surface of the frosted glass must not be oiled.
A.5.3 Analysis steps
Weigh about 5g of uniformly mixed sample, accurate to 0.001 g, placed in a 250 mL iodine bottle, and add 30 mL of glacial acetic acid mixed with chloroform.
The solution was shaken to dissolve the sample sufficiently. Add 0.5 mL of saturated potassium iodide solution, tightly cover the reaction for 1 min, and gently shake the iodine bottle during the reaction.
3 times. Then immediately add 30 mL of water and 0.5 mL of starch indicator solution, titrate with sodium thiosulfate standard titration solution, shake while shaking, near
At the end point, continuously shake all the iodine from the solvent layer, and add the sodium thiosulfate standard titration solution dropwise until the solution blue disappears.
That is the end point. At the same time, the blank test should be carried out. When the standard sodium titration solution of sodium thiosulfate consumed by the blank test exceeds 0.1 mL, the reagent should be replaced.
The sample was re-measured.
A.5.4 Calculation of results
The peroxide value is expressed in w3 and the value is expressed in milliequivalents (meq/kg) of active oxygen per kilogram, calculated according to formula (A.3):
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GB 28401—2012
w 3 
In the formula:
1000  ( V  V 0 )  c
m 3
„„„„„„„„„„„„„„„ (A.3)
V——The volume of the standard titration solution of sodium thiosulfate consumed in the titration sample, in milliliters (mL); V0——the volume of the standard titration solution of sodium thiosulfate consumed in the titration blank, in milliliters (mL) ; c - the exact value of the concentration of sodium thiosulfate standard titration solution, in moles per liter (mol / L); m3 - the value of the sample mass, in grams (g);
1000 - conversion factor.
The experimental results are based on the arithmetic mean of the parallel determination results. The absolute difference between two independent determinations obtained under repeatability conditions shall not exceed 5% of the arithmetic mean.

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