Glycine CAS 56-40-6 (H-Gly-OH) Kev Ntsuas 98.5 ~ 101.5% Lub Hoobkas Zoo

USP35-NF30
DEFINITION
Glycine muaj NLT 98.5% thiab NMT 101.5% ntawm glycine (C2H5NO2), suav ntawm lub hauv paus qhuav.
IDENTIFICATION
A. INFRARED ABSORPTION <197M>
QHIA
• KEV PAB CUAM
Qauv: 150 mg ntawm Glycine
Ntim: 100 mL ntawm glacial acetic acid
Titrimetric system
(Saib Titrimetry <541>.)
Hom: Direct titration
Titrant: 0.1 N rau chloric acid VS
Endpoint detection: Visual
Kev Ntsuam Xyuas: Dissolve cov qauv hauv 100 mL ntawm glacial acetic acid, thiab ntxiv 1 poob ntawm crystal violet TS.Titrate nrog Titrant mus rau qhov kawg ntsuab.Ua qhov kev txiav txim siab Blank.
Xam cov feem pua ​​​​ntawm glycine (C2H5NO2) hauv cov qauv coj mus kuaj:
Result = {[(VS − VB) × N × F]/W} × 100
VS = Titrant ntim tau noj los ntawm Sample (mL)
VB = Titrant ntim tau noj los ntawm Blank (mL)
N = qhov tseeb normality ntawm Titrant (mEq/mL)
F = equivalency factor, 75.07 mg/mEq
W = Sample nyhav (mg)
Kev lees txais: 98.5% -101.5% ntawm lub hauv paus qhuav
IMPURITIES
• RESIDUE ON IGNITION <281>: NMT 0.1%
• chloride thiab sulfate, chloride <221>
Standard tov: 0.10 mL ntawm 0.020 N hydrochloric acid
Qauv: 1 g ntawm Glycine
Kev lees txais: NMT 0.007%
• chloride thiab sulfate, sulfate <221>
Standard tov: 0.20 mL ntawm 0.020 N sulfuric acid
Qauv: 3 g ntawm Glycine
Kev lees txais: NMT 0.0065%
• Hnyav hlau, Txoj Kev I <231>: NMT 20 ppm
• Hnyav hlau, Txoj Kev I <231>: NMT 20 ppm
Cov qauv tshuaj: 100 mg / mL ntawm Glycine
Kev Ntsuam Xyuas: Boil 10 mL ntawm cov qauv tshuaj rau 1 min, thiab tso tseg rau 2 h.
Kev lees txais cov txheej txheem: Cov tshuaj zoo li pom meej thiab zoo li txawb li 10 mL ntawm tib cov tshuaj uas tsis tau boiled.
TSEEM CEEB
• LOSS RAU DRYING <731>: Qhuav ib qho qauv ntawm 105 ° rau 2 h: nws poob NMT 0.2% ntawm nws qhov hnyav.
TSEEM CEEB
• PACKAGING THIAB STORAGE: Khaws rau hauv cov thawv kaw kom zoo.
• USP REFERENCE STANDARDS <11>
USP Glycine RS

Japanese Pharmacopoeia JP17
Glycine, thaum qhuav, muaj tsawg dua 98.5% ntawm Glycine (C2H5NO2).
Kev piav qhia Glycine tshwm sim li dawb, muaju los yog crystalline hmoov.Nws muaj qab zib.Nws yog dawb do soluble nyob rau hauv dej thiab formic acid, thiab xyaum insoluble nyob rau hauv ethanol (95).Nws qhia tau hais tias siv lead ua polymorphism.
Kev txheeb xyuas Kev txiav txim siab qhov infrared absorption spectrum ntawm Glycine, yav tas los qhuav, raws li qhia hauv cov txheej txheem potassiumbromide disk nyob rau hauv Infrared Spectrophotometry <2.25>, thiab sib piv cov spectrum nrog Reference Spec-trum: ob qho tib si spectra pom zoo sib xws ntawm kev nqus ntawm tib lub nthwv dej.Yog tias muaj qhov sib txawv ntawm qhov spectra, yaj Glycine hauv dej, evaporate cov dej todryness, thiab rov ua qhov kev sim nrog cov seem.
pH <2.54> Dissolve 1.0 g ntawm Glycine hauv 20 mL dej: pH ntawm cov tshuaj yog nyob nruab nrab ntawm 5.6 thiab 6.6.
Purity
(1) Clarity thiab xim ntawm kev daws-Dissolve 1.0 gof Glycine hauv 10 mL dej: cov tshuaj yog ntshiab thiab xim-tsawg.
(2) Chloride <1.03>- Ua qhov kev sim nrog 0.5 g ntawm Glycine.Npaj cov tshuaj tswj nrog 0.30 mL ntawm 0.01mol / L hydrochloric acid VS (tsis ntau tshaj 0.021%)
(3) Sulfate <1.14>- Ua qhov ntsuas nrog 0.6 g ntawm Glycine.Npaj cov tshuaj tswj nrog 0.35 mL ntawm 0.005mol / L sulfuric acid VS (tsis ntau tshaj 0.028z).
(4) Ammonium <1.02>-Ua qhov kev sim siv 0.25 g ntawm Glycine.Npaj cov tshuaj tswj nrog 5.0 mL ntawm Standard Ammonium Solution (tsis ntau tshaj 0.02%).
(5) Heavy Metals <1.07>-Tau nrog 1.0 g ntawm Glycine raws li Txoj Kev 1, thiab ua qhov kev sim.Npaj cov tshuaj tswj nrog 2.0 mL ntawm Standard Lead Solution (tsis ntau tshaj 20 ppm).
(6) Arsenic <1.11>-Npaj cov tshuaj ntsuam xyuas nrog 1.0 gof Glycine raws li Txoj Kev 1, thiab ua qhov kev sim (tsis ntau tshaj 2 ppm).
(7) Lwm Yam Khoom - Dissolve 0.10 g ntawm Glycine hauv 25mL dej thiab siv cov tshuaj no ua cov qauv tshuaj.Pipet 1 mL ntawm cov qauv tov, ntxiv dej kom raws nraim 50 mL.Pipet 5 mL ntawm cov tshuaj no, ntxiv dej kom ua tiav 20 mL, thiab siv cov tshuaj no raws li cov qauv kev daws teeb meem.Ua qhov kev sim nrog cov kev daws teeb meem raws li qhia hauv Thin-txheej Chromatography <2.03>.Spot 5mL txhua tus qauv kev daws teeb meem thiab cov qauv kev daws teeb meem ntawm ib lub phaj ntawm silica gel forthin-txheej chromatography.Tsim lub phaj nrog sib tov ntawm 1-butanol, dej thiab acetic acid (100) (3: 1: 1) mus rau qhov deb li ntawm 10 cm, thiab qhuav lub phaj ntawm 80 ℃ rau 30 feeb.Txau ib qho kev daws teeb meem ntawm ninhydrin hauv acetone (1 hauv 50), thiab ua kom sov ntawm 80 ℃ rau 5 feeb: qhov chaw uas tsis yog qhov chaw tseem ceeb ntawm cov qauv tshuaj tsis yog khaus ntau dua li qhov chaw los ntawm cov qauv kev daws teeb meem.
Poob rau ziab <2.41> Tsis ntau tshaj 0.30% (1 g, 105 ℃, 3 teev).
Residue ntawm Ignition <2.44> Tsis ntau tshaj 0.10% (1g).
Assay Weigh kom meej txog 80 mg ntawm Glycine, yav tas los qhuav, yaj hauv 3 mL ntawm formic acid, ntxiv 50 mL ntawm acetic acid (100), thiab titrate <2.50> nrog 0.1 mol / L perchloric acid VS (potentiometric titration).Ua ib qho kev txiav txim siab dawb huv, thiab ua kom muaj kev kho qhov tsim nyog.
Txhua mL ntawm 0.1 mol / L perchloric acid VS＝7.507 mg ntawm C2H5NO2
Containers thiab cia Containers-Zoo-kaw ntim.