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National Food Safety Standard -- Food Additives -- Lactic acid fatty acid glycerides
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GB 1886.93-2015
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Basic data | Standard ID | GB 1886.93-2015 (GB1886.93-2015) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- Lactic acid fatty acid glycerides | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 7,727 | | Date of Issue | 2015-09-22 | | Date of Implementation | 2016-03-22 | | Regulation (derived from) | PRC National Health and Family Planning Commission 2015 No.8 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China |
GB 1886.93-2015: National Food Safety Standard -- Food Additives -- Lactic acid fatty acid glycerides ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(National food safety standards for food additives lactic acid fatty acid glycerides)
National Standards of People's Republic of China
National Food Safety Standard
Food additive lactic acid fatty acid glycerides
Issued on. 2015-09-22
2016-03-22 implementation
People's Republic of China
National Health and Family Planning Commission released
National Food Safety Standard
Food additive lactic acid fatty acid glycerides
1 Scope
This standard applies to food additive lactic acid fatty acid glycerides.
2 Technical Requirements
2.1 Sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Table 1 Sensory requirements
Project requires test methods
State soft to hard waxy solid
Take the right amount of sample is placed in a clean, dry white porcelain dish, self
Observed under natural light state
2.2 Physical indicators
Physical and chemical indicators should be consistent with the provisions of Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Water, w /% claimed to meet the GB/T 6283
Acid value (in dollars KOH)/(mg/g) in line with claims in Appendix A A.3
Residue on ignition, w /% ≤ 0.1 GB/T 9741
Free glycerol, w /% in line with claims in Appendix A A.4
1- monoglyceride content, w /% in line with claims A.5 in Appendix A
Total lactic acid, w /% in line with claims A.6 in Appendix A
Unsaponifiables, w /% ≤ 2.0 GB/T 5535.1 ether extraction
Lead (Pb)/(mg/kg) ≤ 0.5 GB 5009.12
Appendix A
Testing method
A.1 General Provisions
This standard reagents and water in the absence of other specified requirements, refer to the three water analytical reagent and GB/T 6682 regulations. test
The required 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 of the preparation. 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 can be dispersed in water, soluble in hot isopropyl alcohol, xylene, and cottonseed oil.
A.2.2 Take the sample solution 1mLA.6.3, placed in a 25mL test tube with stopper, was added 0.1mL copper sulfate solution (1g five
Water copper sulfate dissolved in 25mL of water) and 6mL sulfuric acid, mix well. Loosely stoppered, heated in a boiling water bath pot 5min, then
It was cooled in an ice-water bath for 5min. After removal from the ice bath, was added a solution of phenylphenol 0.1mLρ- (75mgρ- phenyl-soluble phenol
5mL1mol/L sodium hydroxide solution) and mix. 1min allowed to stand at room temperature and then heated in a boiling water bath pot 1min. Dark solution
Blue-purple, prove the presence of lactic acid.
A.3 acid value (in dollars KOH) Determination
A.3.1 Reagents and materials
A.3.1.1 ethanol. 95%.
A.3.1.2 potassium hydroxide standard solution. 0.1mol/L.
A.3.1.3 phenolphthalein indicator solution. 1%.
A.3.2 Analysis step
Weigh 10g sample (accurate to 0.001g) placed in a conical flask, add 50mL neutral hot ethanol (added to the heated ethanol
2mL phenolphthalein indicator solution with 0.1mol/L potassium hydroxide standard solution to a reddish color does not fade and maintain 30s) to dissolve the sample, with
0.1mol/L potassium hydroxide standard solution titration to reddish and maintain 30s does not fade as the end point.
A.3.3 Calculation Results
Acid value (in dollars KOH) mass fraction w1, according to equation (A.1) Calculated.
w1 =
V × c × M
m × 1000 ×
100% (A.1)
Where.
V --- volume of potassium hydroxide consumed in the titration standard solution, in milliliters (mL);
C --- concentration of standard solution of potassium hydroxide, in units of moles per liter (mol/L);
--- The M molar mass of potassium hydroxide in grams per mole (g/mol), [M (KOH) = 56.1];
M --- the quality of the sample, in grams (g).
A.3.4 allowable difference
The test results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone
Li measurement results and the arithmetic average of the absolute difference of not more than 0.2mg/g.
A.4 Determination of free glycerol
A.4.1 Reagents and materials
A.4.1.1 acetic acid. chemically pure.
A.4.1.2 chloroform. chemically pure, and should meet the following conditions. Take three 500mL flasks, acid-soluble periodate were added 20mL
Liquid, in which the two conical flask 50mL chloroform and 10mL water, another was added 50mL of water, and then further each conical flask
Potassium iodide solution was added 20mL uniformly mixed, placed 1min ~ 5min, according to A.4.2 Analysis step with 0.1mol/L sodium thiosulfate standard
Standard solution titration with chloroform and chloroform without dropping quantitative difference does not exceed 0.5mL.
A.4.1.3 periodic acid solution. dissolve 2.7g periodic acid in a mixture of 50mL and 950mL of acetic acid in water, stored in the dark in a clean stoppered
Glass bottles.
A.4.1.4 potassium iodide solution. mass fraction of 15%.
A.4.1.5 sodium thiosulfate standard solution. 0.1mol/L.
A.4.1.6 starch indicator solution. 0.5%.
A.4.2 Analysis step
First sample melted (its melting temperature does not exceed 10 ℃) and mixed thoroughly. Accurately weighed sample 0.2g (accurate to 0.0001g),
Add 100mL beaker, add chloroform 25mL dissolved. The solution was transferred to a separatory funnel, separate shower with 25mL chloroform
Wash the beaker and then with 25mL water cleaning, all washes were added to a separatory funnel. Gasser sealed, strong shaking 30s ~ 60s, then static
Chloroform and the aqueous phase is set so that stratification (eg formation of milky, may be breaking ice acetic acid 1mL ~ 2mL). The aqueous layer was transferred to 500mL
Iodine bottle, and then were extracted twice with a chloroform solution of 25mL of water. The aqueous phase is extracted concentrate 500mL iodine bottle, add
20.0mL periodic acid solution, and water instead of the sample with 75mL twice a blank test, standing 30min ~ 90min. In each cone
Each bottle plus 15mL15% potassium iodide solution, then placed 1min ~ 5min, add 100mL water, 0.1mol/L sodium thiosulfate standard
Titration solution, titration was stirred using a magnetic stirrer to keep the solution was thoroughly mixed and faded to brown iodine, add 2mL starch indicator
Liquid and continue to drop until the blue fade.
A.4.3 Calculation Results
Free glycerol mass fraction w2, according to equation (A.2) Calculated.
w2 =
(V0-V1) × c × M
m × 1000 ×
100% (A.2)
Where.
Volume V0 --- blank titration consumption of sodium thiosulfate standard solution, in milliliters (mL);
Volume V1 --- sample titration consumption of sodium thiosulfate standard solution, in milliliters (mL);
c --- sodium thiosulfate standard solution concentration, in units of moles per liter (mol/L);
The molar mass of the M glycerol --- 1/40 in grams per mole (g/mol), M
40C3H8O3
÷ = 2.30é
êê
úú;
M --- the quality of the sample, in grams (g).
A.4.4 allowable difference
The test results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone
Li measurement results and the arithmetic average of the absolute difference of not more than 0.2%.
Determination A.5 1- monoglyceride content
A.5.1 Reagents and materials
A.5.1.1 periodic acid solution. dissolve 2.7g periodic acid in a mixture of 50mL and 950mL of acetic acid in water, stored in the dark in a clean stoppered
Sub-glass bottle.
A.5.1.2 Potassium Iodide. Chemical pure, 15% solution.
A.5.1.3 sodium thiosulfate standard solution. 0.1mol/L.
A.5.1.4 acetic acid. chemically pure.
A.5.1.5 starch indicator solution. 0.5%.
A.5.1.6 chloroform. chemically pure, and should meet the following conditions. Take three 500mL flasks, acid-soluble periodate were added 20mL
Liquid, in which the two conical flask 50mL chloroform and 10mL water, another was added 50mL of water, and then further each conical flask
Potassium iodide solution was added 20mL uniformly mixed, placed 1min ~ 5min, according to A.4.2 Analysis step with 0.1mol/L sodium thiosulfate standard
Standard solution titration with chloroform and chloroform without dropping quantitative difference does not exceed 0.5mL.
A.5.2 Analysis step
First sample melted (its melting temperature does not exceed 10 ℃) and mixed thoroughly. Accurately weighed sample 0.2g (accurate to 0.0001g),
Add 100mL beaker, add chloroform 25mL dissolved. The solution was transferred to a separatory funnel, separate shower with 25mL chloroform
Wash the beaker and then with 25mL water cleaning, all washes were added to a separatory funnel. Gasser sealed, strong shaking 30s ~ 60s, then static
Chloroform and the aqueous phase is set so that stratification (eg formation of milky, may be breaking ice acetic acid 1mL ~ 2mL). The aqueous layer was transferred to 500mL
Iodine bottle, and then were extracted twice with a chloroform solution of 25mL of water. The chloroform solution of iodine after extraction into 500mL bottle
While with 50mL chloroform and 10mL water twice a blank test. Periodate acid were added 20mL gentle agitation, and then allowed to stand
30min ~ 90min. In each flask were added to each 15mL15% potassium iodide solution, then placed 1min ~ 5min, add 100mL of water,
Performed using standard sodium thiosulfate solution 0.1mol L/titration, titration was stirred using a magnetic stirrer to keep the solution mixed thoroughly to iodine
After fade brown, add 2mL starch indicator solution and continue to drop until the blue fade.
A.5.3 Calculation Results
1- monoglyceride content mass fraction w3, according to equation (A.3) Calculated.
w3 =
(V0-V1) × c × M
m × 1000 ×
100% (A.3)
Where.
Volume V0 --- blank titration consumption of sodium thiosulfate standard solution, in milliliters (mL);
Volume V1 --- sample titration consumption of sodium thiosulfate standard solution, in milliliters (mL);
c --- sodium thiosulfate standard solution concentration, in units of moles per liter (mol/L);
M --- glycerol monostearate 1/20 molar mass, in grams per mole (g/mol), M
20C21H42O4
÷ = 17.927é
êê
úú;
M --- the quality of the sample, in grams (g).
A.5.4 allowable difference
The test results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone
Li measurement results and the arithmetic average of the absolute difference of not more than 1.0%.
A.6 Determination of total lactic acid
A.6.1 Reagents and materials
A.6.1.1 potassium hydroxide ethanol solution. 0.5mol/L.
A.6.1.2 methyl red.
A.6.1.3 hydrochloric acid solution. 0.5mol/L.
A.6.1.4 hexane.
A.6.1.5 phenolphthalein test.
A.6.1.6 potassium hydroxide solution. 0.1mol/L.
A.6.2 Instruments and Equipment
Air-cooled condenser.
A.6.3 Analysis step
Sample melted sample weight, the equivalent of 140mg ~ 170mg lactic acid. The sample was placed in a 250mL Erlenmeyer flask were added
20mL0.5mol/L potassium hydroxide ethanol solution, connecting a length of at least 65cm in the air-cooled condenser, refluxed for 30min. Simultaneously,
In another empty Erlenmeyer flask, 0.5mol/L potassium hydroxide solution was added to an equal volume of ethanol, blank control experiment. Then, in each
Flask was added 20mL of water, to separate the condenser, the solution was evaporated to a volume of 20mL, cooled to 40 ℃. In each flask was added methyl
Gihon test solution with 0.5mol L solution of hydrochloric acid/titration blank. Meanwhile 0.5mol/L hydrochloric acid solution was spin sample bottle, adding an equal volume.
Was added 50mL of n-hexane in each flask vigorously rotating sample bottle, to dissolve fatty acids and the quantitative contents of each flask was divided
Do not transferred to a 250mL separating funnel, shake 30s. Collecting the aqueous phase to a 300mL Erlenmeyer flask, washed with 50mL of n-hexane solution
Solutions were combined and washed with conical flask was placed in the start phase aqueous solution, n-hexane solution discarded. With 0.1mol/L potassium hydroxide solution
Titration with phenolphthalein test indicator to do, until the solution was pink, holding 30s do not fade, is the titration end point.
Note. The sample solution was kept after the final titration experiments for the above identification.
A.6.4 Calculation Results
Total lactic acid mass fraction w4, according to equation (A.4) Calculated.
w4 =
M × V-V0 () × c
m × 1000 ×
100% (A.4)
Where.
Molar mass of the M 1/10 --- lactic acid units of grams per mole (g/mol), M
10C3H6O3
÷ = 9.008é
êê
úú;
Volume of 0.1mol/L potassium hydroxide solution consumed the V --- titration sample solution, in milliliters (mL of);
V0 blank solution consumed in the titration --- 0.1mol/L solution of potassium hydroxide by volume in milliliters (mL of);
C --- concentration of potassium hydroxide, in units of moles per start (mol/L);
M --- the quality of the sample, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail.
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