GB 1903.1-2015National Food Safety Standard -- Food Nutrition Enhancer -- L-Lysine monohydrochloride (English PDF)

2.1 Chemical Name

L-2,6- two-aminocaproic acid hydrochloride Formula 2.2 C6H14N2O2 · HCl

2.3 Formula

2.4 Relative molecular mass

182.65 (according to 2007 international relative atomic mass)

3.1 Sensory requirements

Sensory requirements shall comply with the requirements of Table 1.

Table 1 Sensory requirements

Project requires test methods Color White State crystal or crystalline powder, no visible impurities Odour odorless Take the right amount of sample is placed in a clean, dry white porcelain dish, self Observe the color and state of natural light, smell the smell

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 20D 20.3 ° ~ 21.5 ° Appendix Specific rotation [alpha] A in A.3 Content (dry matter basis), w /% 98.5 ~ 101.5 Appendix A A.4 Transmittance /% >= 95.0 Appendix A A.5 Loss on drying, w /% <= 1.0 A.6 in Appendix A pH 5.0 ~ 6.0 in Appendix A A.7 Ash, w /% <= 0.2 Appendix A A.8 Lead (Pb)/(mg/kg) <= 5.0 GB 5009.12 Total arsenic (As)/(mg/kg) <= 1.0 GB 5009.11 Salt, w /% <= 0.02 A.9 in Appendix A 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 prepared. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution.

A.2 Identification Test Confirm A.2.1 amino acids A.2.1.1 Reagents and materials Ninhydrin solution. 1g/L.

A.2.1.2 Test procedure A sample was weighed 0.1g (accurate to 0.01g), dissolved in water and diluted to 100mL. Take 5mL of this solution, add 1mL ninhydrin solution Fluid, mixed, heated in a water bath 3min.

A.2.1.3 results found If the final solution was purple, it is recognized as an amino acid.

Confirm A.2.2 chloride A.2.2.1 Reagents and materials A.2.2.1.1 nitrate.

A.2.2.1.2 silver nitrate solution (0.1mol/L). Weigh 17.5g of silver nitrate, dissolved in water and diluted to 1000mL.

A.2.2.1.3 aqueous ammonia solution (10%).

A.2.2.2 Test procedure Weigh the sample 1g (accurate to 0.1g), dissolved in water. To this solution was added silver nitrate solution (A.2.2.1.2) 5mL, and mix.

A.2.2.3 results found If immediately generated a white emulsion precipitation, the precipitate insoluble in nitric acid, and slightly soluble in excess of ammonia, it is determined chlorides.

A.2.3 solubility

Soluble in water, very slightly soluble in ethanol, insoluble in ether.

A.3 Determination of specific optical rotation [alpha] 20D of A.3.1 Reagents and materials Hydrochloric acid solution. 6mol/L.

A.3.2 Instruments and Equipment Automatic polarimeter.

A.3.3 Analysis step

He said drying to constant weight of the sample 5g (accurate to 0.0001g), was dissolved in hydrochloric acid solution taken at 105 °C ± 2 °C, and transferred to 50mL capacity Flask, hydrochloric acid solution to near the mark, the temperature of the solution was adjusted to 20 °C, with a hydrochloric acid solution volume to 50mL, and mix. With the long 2dm Optical tube measuring its optical rotation. Also recorded sample liquid temperature.

A.3.4 Calculation Results the use of the sodium D line spectrum, 2dm optical tube when the sample was measured at 20 °C, according to equation (A.1) sample calculation L- lysine monohydrochloride Specific rotation.

[Alpha] 20D =

a1 × 50

Where.

a1 --- 20 °C sample solution when measured optical rotation in degrees (°);

2 --- Polarimetry length in decimeters (DM);

m --- called lysine hydrochloride L- taken after drying mass in grams (g).

When using the sodium D line spectrum, 2DM offer Polarimetry, when the sample liquid temperature t °C measured, according to equation (A.2) and formula (A.3) calculated L- lysine hydrochloride Specific rotation acid sample.

[Alpha] tD =

a2 × 50

[Alpha] 20D = [alpha] tD -0.02 (20-t) (A.3) where.

Measured sample solution a2 --- t °C when optical rotation in degrees (°);

2 --- Polarimetry length in decimeters (DM);

m --- Weigh quality L- lysine hydrochloride, in units of grams (g);

0.02 --- L- lysine monohydrochloride temperature correction coefficient;

t --- measuring the temperature of the sample solution, in degrees Celsius (°C).

The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Value should not be more than 0.3% of the arithmetic mean.

A.4 Determination of content (dry matter basis) A.4.1 Reagents and materials A.4.1.1 acid.

A.4.1.2 glacial acetic acid.

A.4.1.3 mercuric acetate - acetic acid solution. Weigh 6.0g mercuric acetate, acetic acid plus 100mL dissolve, and mix.

A.4.1.4 alpha- naphthol phenyl alcohol indicator solution. Weigh 0.2g phenyl alpha- naphthol methanol, add 100mL glacial acetic acid dissolve, mix and set aside.

A.4.1.5 perchloric acid standard titration solution. c (HClO4) = 0.1mol/L.

A.4.2 Analysis step

Weigh at 105 °C ± 2 °C drying to constant weight of the sample 0.2g (accurate to 0.0001g), add formic acid 3mL, dissolved, ice acetic acid 50mL, mercuric acetate - acetic acid solution 5mL, then add 10 drops of alpha- naphthol benzhydrol indicator solution, titration with perchloric acid standard solution titration to dissolve VIS green, record volume consumed perchloric acid standard titration solution, while a blank titration test. If the sample is titrated with perchloric acid droplets standards when the temperature of the solution set difference exceeds 10 °C, should be re-calibrated concentration of perchloric acid solution, calibration temperature If a sample is titrated with perchloric acid solution when Difference does not exceed 10 °C, according to equation (A.4) calibration concentration perchloric acid solution.

1 0.0011 × (t1-t0)

Where.

Perchloric acid concentration of the solution during C0 --- calibrated in units of moles per liter (mol/L);

0.0011 --- expansion coefficient of acetic acid;

t1 perchloric acid solution temperature when --- titration sample, in degrees Celsius (°C);

t0 --- perchloric acid solution temperature during calibration, in degrees Celsius (°C).

A.4.3 Calculation Results L- lysine hydrochloride (dry matter basis) of the mass fraction w1, according to equation (A.5,) Calculated.

c1 × (V-V0) × M

m1 × 1000 ×

100% (A.5)

Where.

Concentration c1 --- perchlorate standard solution, the unit is mol per liter (mol/L);

V --- sample titration consumption of perchloric acid standard titration solution volume in milliliters (mL);

V0 --- blank titration consumed perchloric acid standard titration solution volume in milliliters (mL);

M --- L- lysine hydrochloride molar mass in grams per mole (g/mol), M 2C6H14N2O2

· HCl

÷ = 91.32é

M1 --- the quality of the sample, in grams (g);

1000 --- conversion factor.

The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Value should not exceed 0.2% of the arithmetic mean.

A.5 Determination of light transmittance A.5.1 Instruments and Equipment A.5.1.1 flask. 100mL.

A.5.1.2 Spectrophotometer.

A.5.2 Analysis step

Weigh 5g sample (accurate to 0.01g), dissolved in water, dilute to 100mL, shake. With a 1cm cuvette, with water as the blank, Determination of light transmittance of the sample solution at a wavelength of 430nm, the readings are recorded.

The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Value should not exceed 0.2% of the arithmetic mean.

A.6 Determination of loss on drying A.6.1 Instruments and Equipment A.6.1.1 electric oven. 105 °C ± 2 °C.

A.6.1.2 analytical balance. a sense of the amount of 0.1mg.

A.6.1.3 weighing bottle. phi50mm × 30mm.

A.6.1.4 drier. with color gel desiccant.

A.6.2 Analysis step

Weigh the sample 2g (accurate to 0.0002g) to have been baked to constant mass weighing bottle, placed in 105 °C ± 2 °C electric oven baking Dry 3h, stamp removed, placed in the dryer, cooling 30min, weighing.

A.6.3 Calculation Results Loss on drying w2, according to equation (A.6) Calculated.

m2-m3

m3-m0 ×

100% (A.6)

Where.

m2 --- drying bottle quality before adding the sample in grams (g);

m3 --- After drying bottle plus sample mass, in grams (g);

Mass m0 --- weighing bottle in grams (g).

The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Value should not exceed 1% of the arithmetic mean.

A.7 pH measurement

A.7.1 Instruments and Equipment Acidity (pH meter).

A.7.2 Analysis step

Weigh the sample 5g (accurate to 0.02g), add water to dissolve 50mL, with acidimeter solution pH.

The difference between the same two samples of the test results does not exceed 0.02pH.

A.8 Determination of ash A.8.1 Reagents and materials Sulfuric acid. 98%.

A.8.2 Instruments and Equipment A.8.2.1 oven temperature. 550 °C ± 25 °C.

A.8.2.2 porcelain crucible.

A.8.2.3 dryer. color gel.

A.8.3 Analysis step

To constant weight by burning crucible weighed sample 1g (accurate to 0.0001g), placed on a hot plate heated slowly, carefully charring cooling. plus 1mL ~ 2mL of sulfuric acid, heated until smoking, then moved into the high-temperature furnace, burning at 550 °C ± 25 °C 2h, until the furnace temperature dropped to 300 °C left Right, take out the crucible, covered, in a desiccator, cooled to room temperature, and weighed. And then transferred to a high temperature burning furnace 1h, removed, cooled, weighed, heavy Repeat the above operation until constant weight.

A.8.4 Calculation Results Ash w3, according to equation (A.7) calculated as follows.

m6-m4

m5-m4 ×

100% (A.7)

Where.

m6 --- ignition to constant weight of the crucible plus the quality of residue on ignition in grams (g);

m4 --- crucible mass in grams (g);

Crucible plus mass of the sample before m5 --- burning in grams (g).

The absolute difference between the same two samples of the test results should not exceed 1% of the arithmetic mean.

A.9 Determination of ammonium A.9.1 Reagents and materials A.9.1.1 magnesia.

A.9.1.2 sodium hydroxide solution. 1mol/L.

A.9.1.3 hydrochloric acid solution. take 23.41mL amount of concentrated hydrochloric acid, diluted with water to 100mL.

A.9.1.4 alkaline potassium mercuric iodide test solution. take potassium iodide 10g, add water to dissolve 10mL, slowly added a saturated aqueous solution of mercury dichloride, with the Added with stirring to the resulting red precipitate is no longer dissolved, the hydrogenation hydroxide 30g, dissolved, coupled with a saturated solution of mercury dichloride and an aqueous solution 1mL 1mL or more, and diluted with an appropriate amount of water to make 200mL, allowed to stand to precipitate, that is, too. The supernatant was poured from the upper application when used.

A.9.1.5 ammonia-free water.

A.9.1.6 Standard chloride solution. Weigh ammonium chloride 31.5mg, set 1000mL volumetric flask, add water to dissolve and dilute to the mark, Shake, that was the equivalent of 10µg per 1mL of ammonium (NH4) solution.

A.9.2 Instruments and Equipment A.9.2.1 retorts. 500mL.

A.9.2.2 Nessler colorimetric tube. 50mL.

A.9.3 Analysis step

Weigh the sample 0.10g, home distillation flask, add ammonia-free distilled water 200mL, plus magnesium oxide 1g, heating distillation, distillate imported salt added Acid solution and 1 drop of ammonia-free distilled water 50mL 5mL Nessler colorimetric tube, up to 40mL distillate, the distillation was stopped, add sodium hydroxide test 5 drops of liquid, add ammonia-free distilled water to 50mL, plus alkaline potassium mercuric iodide test solution 2mL, shake, place 15min, with the standard ammonium chloride solution Control solution 2mL prepared as described above. Color sample solution should not be deeper than the color produced by the control solution.