H-Gly-OMe·HCl CAS 5680-79-5 Glycine Methyl Ester Hydrochloride Assay >99.0%

1. Properties: This product should be white crystalline powder.
2. Assay:
1) Determination of Glycine Methyl Ester Hydrochloride assay
1.1 Method
Under acidic conditions, the sample reacts with a certain amount of silver nitrate, and the excess silver nitrate is revertitrated with ammonium thiocyanate, referring to ammonium ferric sulfate
As indicator, the total chlorine content was determined according to the volume of the standard solution consumed, and the total chlorine content was subtracted from the content of glycine hydrochloride to obtain Glycine Methyl Ester Hydrochloride content.
1.2 Reagents
Dibutyl phthalate;
Nitric acid solution: 2+3;
Silver nitrate standard titration solution: c(AgNO3) = 0.1 mol/L
Ammonium thiocyanate standard titration solution: c(NH4SCN) = 0.1 mol/L
Ammonium ferric sulfate (III) indicator liquid: 80 g/L
1.3 Analysis Procedure
Weigh about 0.5g sample, accurate to 0.0001g. Place in a 250ml conical flask, dissolve in 40ml water, add 10 ml nitric acid solution, Add (50 ± 0.02) mL silver nitrate standard titration solution, 3mL ammonium ferric sulfate indicator solution, 4mL dibutyl phthalate, and thiocyanate Ammonium standard titration solution was titrated until the solution was light brown and remained colourless for 30 s.
1.4 Result calculation
The mass fraction of glycine methyl ester hydrochloric acid content w1, which is expressed as %, is calculated according to Equation (1) :
w1= (c1V1-c2V2)*M/1000/m * 100-w2 *1.126 formula (1)
Where:
V1: Volume of silver nitrate standard titration solution (ml)
V2: Volume of ammonium thiocyanate standard titration solution consumed by titration (ml)
c1: Exact value of silver nitrate standard titration solution (mol/L)
c2: Exact value of ammonium thiocyanate standard titration solution (mol/L)
w2: Mass fraction (%) of glycine hydrochloride content as determined in Section 4.2
M: Molar mass of glycine methyl ester hydrochloride (g/mol)
1.126: Conversion coefficient of glycine hydrochloride to Glycine methyl ester hydrochloride.
The arithmetic mean value of two parallel measurement results was taken as the measurement result, and the absolute difference between the two parallel measurement results was no more than 0.05%.
2) Determination of glycine hydrochloride content
2.1 Method
Using dimethyl yellow as an indicator, the sample was titrated with sodium hydroxide standard titrating solution, and the volume of the solution was titrated according to the consumption of sodium hydroxide standard.
Calculate the glycine hydrochloride content.
2.2 Reagent
Standard titration solution of sodium hydroxide: c (NaOH) = 0.1mol/L
Dimethyl yellow indication liquid: 10 g/L
2.3 Analysis Procedure
Weigh about 5.0 g laboratory sample, accurate to 0.0001g, into a 200 ml beaker, dissolve with 50ml water, and add 5 drops of dimethyl
Yellow indication liquid, with sodium hydroxide standard titration solution titration until the solution from red to orange yellow is the end point
2.4 Result Calculation
The mass fraction w2 of glycine hydrochloride content is expressed as % and calculated according to Equation (2):
w2 =(V/1000)cM/m *100 formula (2)
Where:
V: Volume of sodium hydroxide standard titration solution (mL)
c: Exact value of sodium hydroxide standard titration solution concentration (mol/L)
M: Molar mass of glycine hydrochloride (g/mol)
m: Mass value of the sample (g)
The arithmetic mean value of two parallel measurement results was taken as the measurement result, and the absolute difference between the two parallel measurement results was no more than 0.05%
3. Melting point: According to the method of melting point determination (Chinese Pharmacopoeia 2010 Appendix VIC), the melting point range is 172-178 ºC.
4. Drying weight loss: take this product at 105.0℃ and dry it to constant weight. The weight loss shall not exceed 0.5%.
5. Storage: This product should be refrigerated away from light.