GB 1986-2007Food additive -- Glyceryl mono-and distearate (English PDF)

3.1 Sensory requirements

Milky white or pale yellow waxy solid, free of impurities, odorless and tasteless.

3.2 Physical and Chemical Indicators

Shall comply with the requirements in Table 1.

Table 1 Physical and Chemical Indicators

Item Index

Acid value (in dollars KOH)/(mg/g) <= 5.0 Free glycerol /% <= 7.0 Residue on ignition /% <= 0.5 Arsenic (As)/(mg/kg) <= 2.0 Lead (Pb)/(mg/kg) <= 2.0 Test Method 4 Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682 set forth in the water.

4.1 Sensory test

The sample was placed in a clean, dry white porcelain dish, under natural light, observe its color, smell its flavor.

4.2 Identification Test

A proper amount of sample, add equal parts of water, heated to above the melting point 2 °C ~ 5 °C, and maintained at this temperature, it should form irreversible gels.

4.3 TESTING

4.3.1 an acid value

4.3.1.1 Reagents and materials

a) Ethanol. 95%.

b) potassium hydroxide standard solution. 0.1mol/L, according to GB/T 601 method of preparation.

c) phenolphthalein indicator solution. 1%, prepared according to GB/T 603 methods.

4.3.1.2 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.

4.3.1.3 Calculation Results

Acid value according to equation (1).

Where.

X1 --- acid value (in dollars KOH) in milligrams per gram (mg/g);

Potassium hydroxide standard titration solution volume Vp --- when consumed in milliliters (mL);

--- Ba concentration of standard solution of potassium hydroxide, in units of moles per liter (mol/L);

--- 56.1 mmol of potassium hydroxide mass in grams per millimole (g/mmol);

4.3.1.4 Allowable difference

The results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone Li measurement results and the arithmetic mean of the absolute difference should not exceed 0.2mg/g.

4.3.2 Free glycerol

4.3.2.1 Reagents and materials

a) acetic acid. chemically pure.

b) 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, and the other just add 50mL water, and then further each cone 20mL vial was added potassium iodide solution were uniformly mixed, placed 1min ~ 5min, in accordance with step 4.3.2.2 Analysis 0.1mol/L sodium thiosulfate standard solution titration with chloroform and chloroform without dropping quantitative difference does not exceed 0.5mL.

c) 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.

d) a solution of potassium iodide. mass fraction of 15%.

e) sodium thiosulfate standard solution. 0.1mol/L, according to GB/T 601 method of preparation and calibration.

f) Starch indicator solution. 0.5%, prepared according to GB/T 603 methods.

4.3.2.2 Analysis step

Water monoglyceride method for determining phase extraction (see A.1.2.2) concentrated to 500mL iodine bottle, add 20.0mL high Periodic acid solution, and water instead of the sample with 75mL twice a blank test, standing 30min ~ 90min. In each conical flask each plus 15mL15% potassium iodide solution, then placed 1min ~ 5min, add 100mL water, 0.1mol/L sodium thiosulfate standard solution Titration, was stirred with a magnetic stirrer to maintain the solution was thoroughly mixed and iodine to fade brown, add 2mL starch indicator solution and continue Continued to drop until the blue fade.

4.3.2.3 Calculation Results

Free glycerol content according to equation (2).

(Vp Vp 0- 1) × × 2.30 Ba (2) where.

X2 --- free glycerol content,%;

Volume V0 --- blank titration consumption of sodium thiosulfate standard solution, in milliliters (mL);

1 --- sample volume Vp titration consumption of sodium thiosulfate standard solution, in milliliters (mL);

Ba --- sodium thiosulfate standard solution concentration units per liter (mol/L);

2.30 --- glycerol relative molecular mass divided by 40;

4.3.2.4 Allowable difference

The results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone Li measurement results and the arithmetic mean of the absolute difference should not exceed 0.2%.

4.3.3 Residue on ignition

The method according to GB/T 9741 predetermined measurement sample weighing approximately 5g.

4.3.4 Arsenic

The method according to GB/T 5009.11 predetermined measurement.

4.3.5 Lead

The method according to GB/T 5009.12 predetermined measurement.

5.1 Batch determination

By the production units of product quality inspection departments to determine the lot number in accordance with their respective rules, the final mixing and there is uniformity of mass production Product batch.

5.2 Sampling methods and sample size

In each batch of products at random samples of each batch of sample extract 3% of the number of pieces of packaging, each batch of not less than three packs, each Sample of not less than 100g, the extracted sample rapidly mixed, distributed into two clean, dry bottle, marked on the bottle manufacturing plant, producing Product name, batch number, quantity and date of sampling bottle for examination, a bottle seal retained for future reference.

5.3 Factory inspection

5.3.1 factory inspection items include sensory, free glycerol, acid number three.

5.3.2 Each batch of products should be produced by the plant inspection department by the method specified in this standard test and issued before the factory product certification.

5.4 Type inspection

All items specified in the technical requirements of this standard are type inspection items. Type inspection every six months, or when the following One situation when tested.

--- Raw materials, process large changes;

After --- Discontinued resume production;

--- Factory test results with the usual recording is quite different;

--- Quality Supervision, Inspection agencies or when requested by the user.

5.5 Determine the rules

When all the technical requirements for inspection, test results if an index does not meet the requirements of this standard should be re-double sampling multiplexes Inspection. Review the results even if one does not meet this standard, the entire batch of products as unqualified.

When opposition parties, such as supply and demand for product quality arises, selected by mutual agreement of arbitration institutions, according to test methods specified in this standard of conduct arbitration.

6.1 Mark

Product marking shall meet the requirements of the Ministry of Health [2002] Decree 26 of Chapter IV.

6.2 Packaging

Product packaging shall be approved by the state, and in accordance with relevant hygiene standards of food packaging materials, packaging net weight deviation should be consistent State Administration of Quality Supervision, Inspection and Quarantine Section 75 orders.

6.3 Transport

Products during transport shall not be mixed and carried toxic and hazardous substances and pollution, avoid the sun and rain and so on.

6.4 Storage

The product should be stored in well-ventilated, clean, dry place, not with toxic, hazardous and corrosive and other substances exist.

6.5 Shelf Life

From the date of manufacture, in the case of the above-stated storage conditions, original packaging intact, the shelf life of not less than two years.

Appendix A

(Informative)

Determination of monoglyceride content, melting point, iodine value and saponification value A. 1 monoglyceride content A. 1.1 Gas chromatography (Arbitration Act) A. 1.1.1 Method summary Due to the high boiling point monoglycerides, not directly into the column, otherwise it will clog the column. In this method, the monoglycerides and a silane reagent (BSTFA, TMCS) chemical derivatization reaction to form a volatile silane derivative, reduces the boiling point, you can pass Analysis by gas chromatography.

A. 1.1.2 Reagents and materials

a) pyridine. AR.

b) tetradecane. AR.

c) N, O- bis trimethylsilyl trifluoroacetamide (BSTFA). AR.

d) trimethylchlorosilane (TMCS). AR.

e) Glycerol. AR.

f) palmitic acid, stearic acid, monomyristate, glycerol monopalmitate and glycerol monostearate standards. purity of not less at 99%.

A. 1.1.3 Instruments

a) gas chromatograph.

b) Column. EC-5 capillary column (equivalent to SE-54), column length 30m, an inner diameter of 0.25mm, smear thickness 0.25µm.

c) flame ionization detector (FID).

A. Chromatographic conditions 1.1.4 Reference

a) Oven temperature. initial temperature 120 °C, at a rate of 15 °C/min and the temperature was raised to 340 °C maintained 30min.

b) Inlet temperature. 320 °C.

c) detector temperature. 350 °C.

d) carrier gas. nitrogen (capillary flow rate 1mL/min).

e) the hydrogen. 60mL/min.

f) Air. 500mL/min.

g) Split ratio. 1.10 to 1.50.

h) Injection volume. 1µL ~ 5µL.

A. 1.1.5 Analysis of step

a) Weigh accurately tetradecane and standards for each 100mg placed 10mL volumetric flask, pyridine volume as a standard. Standard package Including palmitic acid, stearic acid, glycerol, monomyristate, glycerol monopalmitate and glycerol monostearate six kinds highest content Substances.

b) accurately weighed 100mg and 600mg tetradecane test samples were placed in 10mL volumetric flask, pyridine volume. The exact amount taken 0.10mL sample solution to 2.5mL screw-capped vials, after adding 0.1mLTMCS violent shake and 0.2mLBSTFA, set 70 °C oven reaction 20min, the test sample was obtained.

c) to be GC reaches the specified conditions, into a mixed standard solution and the test sample was measured.

A. 1.1.6 Calculation Results

a) you can get into the standard response factor R, according to the results of the formula (A.1) Calculated.

Where.

R --- response factor;

As --- standard peak area;

Ad --- internal standard peak area;

b) the sample mass fraction of monoglycerides according to formula (A.2) Calculated.

Where.

X4 --- sample monoglycerides mass fraction,%;

Au --- peak area of component to be measured;

Ad --- internal standard peak area;

R --- response factor.

c) by the above formula were calculated palmitic acid, stearic acid, glycerol, monomyristate, glycerol monopalmitate and monostearate Triglyceride levels. Palmitic acid and stearic acid and the content of free fatty acids; glycerol free glycerol content; monopalmitate Triglyceride and glyceryl monostearate and the total content of monoglyceride content.

A. 1.1.7 allowable difference the results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone Li measurement results and the arithmetic mean of the absolute difference does not exceed 0.5%.

A. 1.2 periodic acid method A. 1.2.1 Reagents and materials

a) 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.

b) potassium iodide. chemically pure, 15% solution.

c) sodium thiosulfate standard solution. 0.1mol/L, prepared according to GB/T 601 methods and calibration.

d) acetic acid. chemically pure.

e) Starch indicator solution. 0.5%, prepared according to GB/T 603 methods.

f) chloroform. chemically pure, and should meet the following conditions. Take three 500mL flasks, acid-soluble periodate were added 20mL Liquid, in which the two flask 50mL chloroform and 10mL water, and the other just add 50mL water, go down to each flask Potassium iodide solution was added 20mL uniformly mixed, placed 1min ~ 5min, according to A. 1.2.2 Analysis of step with 0.1mol/L Sodium thiosulfate standard solution titration with chloroform and chloroform-free titration difference of no more than 0.5mL.

A. 1.2.2 Analysis of step First sample melted (its melting temperature does not exceed 10 °C) 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 solution was extracted after concentrated into the same bottle for measuring iodine Given the content of free glycerol. The chloroform solution of iodine after extraction into a 500mL flask with 50mL chloroform and at the same time 10mL water twice a blank test. Periodate acid were added 20mL gentle agitation, and then allowed to stand for 30min ~ 90min. In each flask each plus 15mL15% potassium iodide solution, then placed 1min ~ 5min, add 100mL water, 0.1mol/L sodium thiosulfate standard solution Titrated solution was stirred with a magnetic stirrer, titration to maintain the mixed solution after the iodine to fade brown, add 2mL starch means it was shown, and continues to drop until the blue fade.

A. 1.2.3 Calculation Results Sample mass fraction of monoglycerides according to formula (A.3) Calculated.

(Vp Vp 0- 1) × × 17.927 Ba (A.3) where.

X5 --- glycerol monostearate mass fraction,%;

Volume V0 --- blank titration consumption of sodium thiosulfate standard solution, in milliliters (mL);

1 --- sample volume Vp titration consumption of sodium thiosulfate standard solution, in milliliters (mL);

--- The amount of Ba concentration of sodium thiosulfate standard solution material, units per liter (mol/L);

17.927 --- glyceryl monostearate molecular weight divided by 20;

A. 1.2.4 allowable difference the results mean of two parallel determination results shall prevail (to one decimal place). Twice under repeated condition alone Li measurement results and the arithmetic mean of the absolute difference of not more than 1.0%.

A. 2 MP

The method according to GB/T 617 predetermined measurement sample weighing about 4g.

A. 3 iodine value

The method according to GB/T 18953 predetermined measurement.

A. 4 saponification value the method according to GB/T 5534 predetermined measurement.