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GB 29951-2013 English PDF

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GB 29951-2013: Food additive -- Citric acid glycerides of fatty acids
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Basic data

Standard ID GB 29951-2013 (GB29951-2013)
Description (Translated English) Food additive -- Citric acid glycerides of fatty acids
Sector / Industry National Standard
Classification of Chinese Standard C53
Classification of International Standard 67.020
Word Count Estimation 10,110
Regulation (derived from) China Food & Drug Administration [2013] No. 234, November, 1, 2013
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China
Summary This standard applies to food additives: citric acid fatty acid glycerides.

GB 29951-2013: Food additive -- Citric acid glycerides of fatty acids

---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.
Food additive-Citric acid glycerides of fatty acids National Standards of People's Republic of China Issued on. 2013-11-29 2014-06-01 implementation National Food Safety Standard Food additive citric acid fatty acid glycerides National Food Safety Standard Food additive citric acid fatty acid glycerides

1 Scope

This standard applies to glycerol with citric acid and obtained by the esterification of edible fatty acids, or by a mixture of single and double glycerides of edible fatty acids and lemon Citric acid obtained by the reaction of a food additive citric acid fatty acid glycerides. It consists of citric acid and mixed esters of edible fatty acids and glycerin composition may contain A small amount of free fatty acids, free glycerol, citric acid and free glycerides odd and even, in whole or in part by sodium hydroxide or potassium hydroxide.

2 formula

Wherein, R1, R2 and R3 is at least one group of citric acid, a fatty acid group, the other may be a citric acid, a fatty acid, or hydrogen.

3 Technical requirements

3.1 Sensory requirements Sensory requirements shall comply with the requirements of Table 1. Table 1 Sensory requirements Project requires test methods White to light brown color, take appropriate sample is placed within the white porcelain plate, observed under natural light Color and oily to waxy Status 3.2 Physical and Chemical Indicators Physical and chemical indicators should be consistent with the provisions of Table 2. Table 2. Physical and chemical indicators Item Index Test Method Sulphated Ash, w /% ≤ 0.5 (and not the product) Appendix A A.3 10 (partially or completely neutralized product) Free glycerol, w /% ≤ 4 Appendix A A.4 Total glycerol, w /% 8 ~ 33 in Appendix A A.5 Total citric acid, w /% 13 ~ 50 in Appendix A A.6 Total fatty acids, w /% 37 ~ 81 in Appendix A A.7 Lead (Pb)/(mg/kg) ≤ 2 GB 5009.12

Appendix A

Testing method A.1 General Provisions Unless otherwise specified in this standard, the use of analytical reagent purity should be more than the standard titration solution, standard solution for measuring impurities, Preparations and products, should be GB/T 601, GB/T 602, the provisions of the preparation of GB/T 603, the test water should be consistent with GB/T 6682-2008 in three water Provisions. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution. A.2 Identification Test Insoluble in cold water, dispersible in water, fat-soluble, insoluble in cold ethanol. A.3 Determination of sulfated ash A.3.1 Analysis step Weigh 2 g samples, accurate to 0.000 1 g, has been placed on firing at 800 ℃ ± 25 ℃ to constant weight of the crucible, adding a small amount of sulfuric acid, slowly Heating until the sample is completely volatilized or charring. Heating was continued to sulfuric acid vapor Yat do, burned to constant weight at 800 ℃ ± 25 ℃ high temperature furnace. A.3.2 Calculation Results Sulfated ash mass fraction w1 according to formula (A.1) Calculated. 0011  mm (A.1) Where. After m1-- mass burning crucible and residue, in grams (g); m0-- crucible mass in grams (g); m-- sample mass, in grams (g). A.4 Determination of free glycerol A.4.1 Reagents and solutions A.4.1.1 glacial acetic acid. A.4.1.2 chloroform. A.4.1.3 periodic acid solution. 5.4 g of periodic acid is dissolved in a mixture of 100 mL of water and 1900 mL of glacial acetic acid, mixing, stored in the dark with Cypriot glass bottles. A.4.1.4 potassium iodide solution. 150 g/L. A.4.1.5 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1 mol/L. A.4.1.6 starch indicator solution. 10 g/L. A.4.2 Analysis step A.4.2.1 Preparation of sample solution First sample melted (its melting point temperature does not exceed 10 ℃), and mix thoroughly. Accurately weigh 1 g sample taken after mixing, to the nearest 0.001 g, Placed 100 mL volumetric flask, add 50 mL of chloroform to dissolve, then add 25 mL of water, stopper closed strongly shaken 30 s ~ 60 s, Then left to make chloroform and the aqueous phase stratification (such as the formation of milky, you can ice acetic acid 3 mL or 4 mL breaking). Glass siphon, The aqueous phase was transferred to another 100 mL volumetric flask. Then respectively 25 mL, 25 mL and 20 mL of water and extracted three times chloroform solution. will After extraction of the water phase concentrated into the same flask, add water to 100 mL, and mix, this is a sample solution. A.4.2.2 Determination Prepare two 500 mL bottles of iodine were added to 50 mL periodic acid solution. Pipette 50 mL sample solution (A.4.2.1), disposed therein A bottle of iodine. Pipette 50 mL of water, placed in another iodine bottle, blank test. After each shake and let stand 30 min ~ 90 min. After each flask were added 20 mL iodine potassium iodide solution, carefully shake, standing in the dark for 1 min ~ 5 min. Then were added 100 mL Water, sodium thiosulfate standard titration solution was titrated were stirred with a magnetic stirrer, titration to maintain the solution thoroughly mixed. Titrated to iodine After the brown subsided, were added to 2 mL of starch indicator solution and continue titration until the solution is the titration end faded blue. A.4.3 Calculation Results Free glycerol content w2 according to formula (A.2) Calculated.     4100010050 2    McVV w (A.2) Where. Volume V0-- blank titration consumption of sodium thiosulfate standard titration solution, in milliliters (mL); Volume aqueous titration V1-- sample consumption of sodium thiosulfate standard titration solution, in milliliters (mL); C-- actual concentration of sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L); M - molar mass of glycerin units of grams per mole (g/mol) [M (C3H8O3) = 92]; m-- sample mass, in grams (g); Volume ratio of 50/100-- sample solution; 1000-- volume conversion factor; 4-- conversion factor. A.5 Determination of Total glycerol A.5.1 Reagents and solutions A.5.1.1 glacial acetic acid. A.5.1.2 chloroform. A.5.1.3 Potassium hydroxide - ethanol solution. 0.5 moL/L. A.5.1.4 periodic acid solution. dissolve 5.4 g of periodic acid in a mixture of 100 mL of water and 1900 mL glacial acetic acid, and stored in the dark glass bottle with stopper in. A.5.1.5 potassium iodide solution. 150 g/L. A.5.1.6 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1 mol/L. A.5.1.7 starch indicator solution. 10 g/L. A.5.2 Instruments and Equipment A.5.2.1 round-bottomed flask. 250 mL. A.5.2.2 reflux condenser. A.5.3 Analysis step A.5.3.1 Preparation of sample solution Weigh a sample of about 2 g, accurate to 0.001 g, placed in a round bottom flask was added 50 mL of potassium hydroxide - ethanol solution. The mixture containing The flask was connected to a reflux condenser, was heated at reflux for 30 min. Each with 3 parts of water Add 25 mL round bottom flask mixture was transferred to a 1 L Volumetric flask, accurately added 99 mL of chloroform and 25 mL of glacial acetic acid, then add about 500 mL of water, shaken vigorously for about 1 min. Diluted with water Diluted to the mark, mix well, let stand stratification. After separation of the aqueous phase to give a sample solution. A.5.3.2 Determination Prepare two 400 mL beaker were added 50 mL periodic acid solution. Pipette 50 mL sample solution (A.5.3.1), placed one Beaker. Pipette 50 mL of water, placed in a separate beaker, blank test. After careful shaking, covered glass dish, allowed to stand for 30 min ~ dark 90 min. In each beaker were added 20 mL potassium iodide solution, after carefully shake and let stand 1 min ~ 5 min. Then were added 100 mL Water, sodium thiosulfate standard titration solution was titrated were stirred with a magnetic stirrer, titration to maintain the solution thoroughly mixed. Titrated to iodine After the brown subsided, were added to 2 mL of starch indicator solution and continue titration until the solution is the titration end faded blue. A.5.4 Calculation Results The total glycerol content mass fraction w3 according to formula (A.3) Calculated.     4100090050 3    McVV w (A.3) Where. Volume V0-- blank titration consumption of sodium thiosulfate standard titration solution, in milliliters (mL); Volume aqueous titration V1-- sample consumption of sodium thiosulfate standard titration solution, in milliliters (mL); C-- actual concentration of sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L); M-- glycerol molar mass in grams per mole (g/mol) [M1 (C3H8O3) = 92]; m-- sample mass, in grams (g); Volume ratio of 50/900-- sample solution; 1000-- volume conversion factor; 4-- conversion factor. A.6 Determination of total citric acid A.6.1 Principle Potassium hydroxide - ethanol solution of the sample is saponified by extraction to remove fatty acids, citric acid in the sample is converted to trimethylsilyl (TMS) Derivatives and analyzed by gas chromatography. A.6.2 Reagents and materials A.6.2.1 heptane. A.6.2.2 hydrochloric acid. A.6.2.3 pyridine. A.6.2.4 trimethylchlorosilane (TMCS). A.6.2.5 hexamethyldisilazane (HMDS). A.6.2.6 N- methyl -N- trimethylsilyl - trifluoroacetamide (MSTFA). A.6.2.7 KOH - ethanol solution. 0.5mol/L. A.6.2.8 tartaric acid solution. 1 mg/mL. A.6.2.9 citric acid control solution. 3 mg/mL. A.6.3 Instruments and Equipment A.6.3.1 reflux condenser. A.6.3.2 rotary evaporator. A.6.3.3 separating funnel. A.6.3.4 gas chromatograph. equipped with a flame ionization detector. A.6.4 Analysis step A.6.4.1 saponification Weigh a sample of about 1 g, accurate to 0.001 g, were placed in a round bottom flask was added 25 mL of potassium hydroxide - ethanol solution containing the mixed The flask was connected with a reflux condenser, refluxed for 30 min. Of the mixture was acidified with hydrochloric acid, in a rotary evaporator and then it was evaporated. A.6.4.2 extraction With no more than 50 mL of water in the flask was concentrated by evaporation (A.6.4.1) quantitatively transferred to a separating funnel with 3 parts of each of 50 mL of heptane extraction, discard the extract, the aqueous layer was transferred to a 100 mL volumetric flask, dilute to the mark with water and after, Mix reserve. A.6.4.3 derived reaction Draw 1 mL solution of tartaric acid and 1 mL solution was A.6.4.2 step was added to a 10 mL round-bottomed flask covered in, And evaporated to dryness. Add 1 mL of pyridine, 0.2 mL of trimethylchlorosilane (TMCS), 0.4 mL hexamethyldisilazane (of HMDS) and 0.1 mL N- methyl -N- Trimethylsilyl - trifluoroacetamide (MSTFA). The flask lid tightly and carefully rotate until completely dissolved solute. The flask was placed in an oven , And it was heated at 60 ℃ 1 h, a sample solution for trimethylsilyl (TMS) derivatized. A.6.4.4 gas chromatographic analysis A.6.4.4.1 Reference GC conditions A.6.4.4.1.1 Column. Glass column, 1.8 m × 2 mm (internal diameter), 10% of the filler of polydimethylsiloxane (DC-200), the carrier Red diatomaceous earth (Q) (180 μm/150 μm); or other equivalent separation columns and chromatographic conditions. A.6.4.4.1.2 column temperature. 165 ℃. A.6.4.4.1.3 Inlet temperature. 240 ℃. A.6.4.4.1.4 detector temperature. 240 ℃. A.6.4.4.1.5 carrier gas. nitrogen. A.6.4.4.1.6 carrier flow rate. 24 mL/min. A.6.4.4.1.7 Injection volume. 5 μL. A.6.4.4.2 Determination In reference A.6.4.4.1 GC conditions, the sample solution (A.6.4.3) chromatographic analysis, record the chromatograms. With 1 mL of citric acid According to the solution instead of 1 mL of sample solution, repeat the above derivative reaction (A.6.4.3) and gas chromatographic analysis. A.6.5 Calculation Results Total citric acid mass fraction w4 according to formula (A.4) Calculated. CS TR CR TS CR 100% AA m AA m        (A.4) Where. ACS-- sample solution chromatogram peak area citric acid; ATR-- citric acid control solution peak area in the chromatogram of tartaric acid; mCR - 1mL quality control citric acid solution of citric acid, in grams (g); 100-- dilution; ATS-- sample solution chromatogram peak area of tartaric acid; ACR-- citric acid control solution peak area in the chromatogram of citric acid; m-- sample mass, in grams (g). A.7 Determination of the total fatty acids A.7.1 Reagents and materials A.7.1.1 anhydrous sodium sulfate. A.7.1.2 hydrochloric acid. A.7.1.3 ether. A.7.1.4 sodium chloride solution. 100 g/L. A.7.1.5 KOH - ethanol. 1 mol/L. A.7.1.6 methyl orange indicator solution. 1 g/L. A.7.2 Instruments and Equipment A.7.2.1 separating funnel. A.7.2.2 reflux condenser. A.7.3 Analysis step Approx. 5 g sample is weighed accurately to 0.001 g, placed in a 250 mL round bottom flask was added 50 mL of potassium hydroxide - ethanol, Reflux for 1 h in a water bath. With 3 portions of 25 mL each of water to the reaction mixture after saponification flask was transferred to a 1L separatory funnel, the plus 5 into drops of methyl orange indicator solution. Be careful addition of hydrochloric acid until the color of the solution turned bright red, then shake to separate the fatty acids. With three each 100 mL of ether extract separated from the fatty acids. The combined extracts were washed with 50 mL of sodium chloride solution was eluted until the eluate is chloride The solution is neutral. The sample solution is dried over anhydrous sodium sulfate, and filtered. Then on a steam bath ether filtrate was evaporated, and then placed 10 min, The residue was weighed. A.7.4 Calculation Results The total fatty acid content w5 according to formula (A.5) Calculated. 015  w (A.5) Where. Quality after m1-- evaporation residue in grams (g); m0-- sample mass, in grams (g).

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