L-Glutamine CAS 56-85-9 (H-Gln-OH) Assay 99.0~101.0% Factory High Quality

Japanese Pharmacopoeia Reference Standards
L-Glutamine [56-85-9]
L-Glutamine, when dried, contains not less than 99.0% and not more than 101.0% of L-Glutamine (C5H10N2O3).
Description L-Glutamine occurs as white, crystals or a crystalline powder. It has a slight characteristic taste
It is freely soluble in formic acid, soluble in water, and practically insoluble in ethanol (99.5)
Identification Determine the infrared absorption spectrum of L-Glutamine as directed in the potassium bromide disk method under Infrared Spectrophotometry <2.25>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wave numbers.
Optical Rotation <2.49> [a]20D:+6.3° to +7.3° Weigh accurately about 2 g of L-Glutamine, previously dried, add 45mL of water, warm to 40℃to dissolve, and after cooling, add water to make exactly 50 mL. Determine the optical rotation of this solution in a 100-mm cell, within 60 minutes.
pH <2.54> The pH of a solution prepared by dissolving 1.0 g of L-Glutamine in 50 mL of water is between 4.5 and 6.0.
Purity
(1) Clarity and color of solution—A solution obtained by dissolving 0.5 g of L-Glutamine in 20 mL of wateris clear and colorless.
(2) Chloride <1.03> —Perform the test with 0.5 g of L-Glutamine. Prepare the control solution with 0.30 mL of 0.01 mol/L hydrochloric acid VS (not more than 0.021%).
(3) Sulfate <1.14>—Perform the test with 0.6 g of L-Glutamine. Prepare the control solution with 0.35 mL of 0.005 mol/L sulfuric acid VS (not more than 0.028z).
(4) Ammonium <1.02>—Perform the test with 0.10 g of L-Glutamine, using the distillation under reduced pressure. Prepare the control solution with 10.0 mL of Standard Ammonium Solution. The temperature of the water bath is45℃ (not more than 0.1%)
(5) Heavy Metals <1.07>—Proceed with 1.0 g of L-Glutamine according to Method 1, and perform the test. Preparethe control solution with 1.0 mL of Standard Lead Solution (not more than 10 ppm).
(6) Iron <1.10>—Prepare the test solution with 1.0 g of L-Glutamine according to Method 1, and perform the test according to Method A. Prepare the control solution with1.0 mL of Standard Iron Solution (not more than 10 ppm)
(7) Related Substances—Dissolve 0.10 g of L-Glutaminein 10 mL of water, and use this solution as the sample solution. Pipet 1 mL of the sample solution, add water to make exactly 10 mL. Pipet 1 mL of this solution, add water tomake exactly 50 mL, and use this solution as the standard solution. Perform the test with these solutions as directed under Thin-layer Chromatography <2.03>. Spot 5mL each of the sample solution and standard solution on a plate of silicagel for thin-layer chromatography. Then develop with amixture of 1-butanol, water and acetic acid (100) (3:1:1) to adistance of about 10 cm, and dry the plate at 80℃ for 30 minutes. Spray evenly a solution of ninhydrin in a mixture of methanol and acetic acid (100) (97:3) (1 in 100) on the plate, and heat at 80℃for 10 minutes: the spot other than the principal spot obtained with the sample solution is not more intense than the spot obtained with the standard solution.
Loss on Drying <2.41> Not more than 0.3% (1 g, 105℃, 3 hours)
Residue on Ignition <2.44> Not more than 0.10%(1 g).
Assay Weigh accurately about 0.15 g of L-Glutamine, previously dried, dissolve in 3 mL of formic acid, add 50 mL of acetic acid (100), and titrate <2.50> with 0.1 mol/L perchloric acid VS (potentiometric titration). Perform a blank determination in the same manner, and make any necessary correction.
Each mL of 0.1 mol/L perchloric acid VS＝14.61 mg of C5H10N2O3
Containers and Storage Containers—Tight containers.

USP Reference Standards <11>-USP Glutamine RS.
Identification, Infrared Absorption <197K>.
Specific Rotation <781S>: between +6.3° and +7.3°, determined at 20℃
Test Solution- In a suitable flask, accurately prepare a solution of about 40mg per ml in water at about 40℃. Cool and dilute with water to volume before use.
Loss on Drying <731>-Dry it at 105℃ for 3 hours; it loses not more than 0.20% of its weight.
Residue on Ignition <281> Not more than 0.30%
Chloride <221>-A 0.7-g portion shows no more chloride than corresponds to 0.50ml of 0.020 N hydrochloric acid: not more than 0.05% is found.
Sulfate <221>-A 0.8-g portion shows no more sulfate than corresponds to 0.25ml of 0.020 N sulfuric acid: not more than 0.03% is found. 
Chromatographic Purity
Adsorbent: 0.25-mm layer of chromatographic silica gel mixture.
Test Solution: 10mg per ml, in water
Standard Solution-Prepare a solution of USP Glutamine RS in water having a known concentration of about 0.05mg per ml.
Application Volume: 5μL
Developing Solvent System: a mixture of butyl alcohol, water, and glacial acetic acid (3:1:1).
Spray Reagent-Dissolve 0.2g of ninhydrin in 100ml of a mixture of butyl alcohol and 2 N acetic acid (95:5)
Procedure-Proceed as directed for thin-layer chromatography under Chromatography <621>, then dry the plate at 80℃ for 30 minutes. Spray the plate with the spray reagent, heat at 80℃ for 10 minutes, and examine under white light:no secondary spot in the chromatogram obtained from the test solution is larger or more intense than the principal spot in the chromatogram obtained from the standrad solution (0.5%)
Organic Volatile Impurities, Method I <467>: Meet the requirements.
Asssy-Transfer about 150mg of Glutamine, accurately weighted, to a 125ml flask , dissolbe in 3ml of formic acid and 50ml of glacial acetic acid, and titrate with 0.1 N perchloric acid VS determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction (see Titrimetry<541>). Each ml of 0.1 N perchloric acid is equivalent to 14.615 mg of C5H10N2O3