L-Glutamine CAS 56-85-9 (H-Gln-OH) Kev Ntsuam Xyuas 99.0 ~ 101.0% Hoobkas Zoo

Japanese PharmacopoeiaCov qauv siv
L-Glutamine [56-85-9]
L-Glutamine, thaum qhuav, muaj tsis tsawg tshaj li 99.0% thiab tsis ntau tshaj 101.0% ntawm L-Glutamine (C5H10N2O3).
Kev piav qhia L-Glutamine tshwm sim li dawb, muaju los yog cov hmoov crystalline.Nws muaj ib tug me ntsis yam ntxwv saj
Nws yog dawb soluble nyob rau hauv formic acid, soluble nyob rau hauv dej, thiab xyaum insoluble nyob rau hauv ethanol (99.5)
Kev txheeb xyuas Kev txiav txim siab qhov infrared absorption spectrum ntawm L-Glutamine raws li qhia nyob rau hauv cov poov tshuaj bromide disk txoj kev nyob rau hauv Infrared Spectrophotometry <2.25>, thiab muab piv cov spectrum nrog cov Reference Spectrum: ob qho tib si spectra qhia zoo sib xws ntawm kev nqus ntawm tib lub nthwv dej.
Kev sib hloov kho qhov muag <2.49> [a]20D: +6.3 ° rau +7.3 ° Qhov hnyav yog kwv yees li 2 g ntawm L-Glutamine, yav tas los qhuav, ntxiv 45mL dej, sov rau 40 ℃ kom yaj, thiab tom qab txias, ntxiv dej los ua. yog 50ml.Txiav txim siab qhov kev hloov kho qhov muag ntawm cov tshuaj no hauv 100-mm cell, hauv 60 feeb.
pH <2.54> Cov pH ntawm cov tshuaj npaj los ntawm dissolving 1.0 g ntawm L-Glutamine hauv 50 mL dej yog nyob nruab nrab ntawm 4.5 thiab 6.0.
Purity
(1) Clarity thiab xim ntawm kev daws - Ib qho kev daws tau los ntawm dissolving 0.5 g ntawm L-Glutamine hauv 20 mL ntawm dej ntshiab thiab tsis muaj xim.
(2) Chloride <1.03>—Ua qhov kev sim nrog 0.5 g ntawm L-Glutamine.Npaj cov tshuaj tswj nrog 0.30 mL ntawm 0.01 mol / L hydrochloric acid VS (tsis ntau tshaj 0.021%).
(3) Sulfate <1.14>—Ua qhov kev sim nrog 0.6 g ntawm L-Glutamine.Npaj cov tshuaj tswj nrog 0.35 mL ntawm 0.005 mol / L sulfuric acid VS (tsis ntau tshaj 0.028z).
(4) Ammonium <1.02>—Ua qhov kev sim nrog 0.10 g ntawm L-Glutamine, siv cov distillation nyob rau hauv lub siab txo.Npaj cov tshuaj tswj nrog 10.0 mL ntawm Standard Ammonium Solution.Qhov kub ntawm cov dej da dej yog 45 ℃ (tsis ntau tshaj 0.1%)
(5) Heavy Metals <1.07>—Tau nrog 1.0 g ntawm L-Glutamine raws li Txoj Kev 1, thiab ua qhov kev sim.Npaj cov tshuaj tswj nrog 1.0 mL ntawm Standard Lead Solution (tsis ntau tshaj 10 ppm).
(6) Hlau <1.10>—Npaj cov tshuaj ntsuam xyuas nrog 1.0 g ntawm L-Glutamine raws li Txoj Kev 1, thiab ua qhov kev sim raws li Txoj Kev A. Npaj cov tshuaj tswj nrog 1.0 mL ntawm Standard Iron Solution (tsis ntau tshaj 10 ppm)
(7) Lwm Yam Tshuaj - Dissolve 0.10 g ntawm L-Glutaminein 10 mL dej, thiab siv cov tshuaj no ua cov qauv tov.Pipet 1 mL ntawm cov qauv tov, ntxiv dej kom raws nraim 10 mL.Pipet 1 mL ntawm cov tshuaj no, ntxiv dej tomake raws nraim 50 mL, thiab siv cov tshuaj no raws li tus qauv tov.Ua qhov kev sim nrog cov kev daws teeb meem no 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 silicagel rau nyias txheej chromatography.Tom qab ntawd txhim kho nrog kev sib xyaw ntawm 1-butanol, dej thiab acetic acid (100) (3: 1: 1) kom deb ntawm li 10 cm, thiab qhuav lub phaj ntawm 80 ℃ rau 30 feeb.Spray tusyees ib tug tov ntawm ninhydrin nyob rau hauv ib tug sib tov ntawm methanol thiab acetic acid (100) (97:3) (1 nyob rau hauv 100) ntawm lub phaj, thiab tshav kub ntawm 80 ℃ rau 10 feeb: qhov chaw uas tsis yog lub hauv paus chaw tau txais nrog lub cov qauv kev daws teeb meem tsis yog khaus ntau dua li qhov chaw tau txais nrog cov qauv kev daws teeb meem.
Poob rau ziab <2.41> Tsis ntau tshaj 0.3% (1 g, 105 ℃, 3 teev)
Residue ntawm Ignition <2.44> Tsis ntau tshaj 0.10% (1 g).
Kev ntsuas qhov hnyav yog kwv yees li 0.15 g ntawm L-Glutamine, 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 paug ib yam nkaus, thiab ua kom muaj kev kho qhov tsim nyog.
Txhua mL ntawm 0.1 mol / L perchloric acid VS＝14.61 mg ntawm C5H10N2O3
Containers thiab Storage Containers-Tight containers.

USP Reference Standards <11>-USP Glutamine RS.
Kev txheeb xyuas, Infrared Absorption <197K>.
Kev sib hloov tshwj xeeb <781S>Qhov kub thiab txias: ntawm +6.3 ° txog +7.3 °, txiav txim siab ntawm 20 ℃
Test Solution- Nyob rau hauv ib lub hwj uas tsim nyog, npaj kom raug cov tshuaj ntawm 40mg ib ml hauv dej ntawm 40 ℃.Txias thiab dilute nrog dej rau ntim ua ntej siv.
Poob rau ziab <731>- Qhuav nws ntawm 105 ℃ rau 3 teev;nws poob tsis ntau tshaj 0.20% ntawm nws qhov hnyav.
Residue ntawm Ignition <281>Tsis ntau tshaj 0.30%
Chloride <221>-Ib qho 0.7-g qhia tias tsis muaj chloride ntau dua li 0.50ml ntawm 0.020 N hydrochloric acid: tsis pub ntau tshaj 0.05%.
Sulfate <221>-Ib qho 0.8-g qhia tias tsis muaj sulfate ntau dua li 0.25ml ntawm 0.020 N sulfuric acid: tsis pub ntau tshaj 0.03%.
Chromatographic Purity
Adsorbent: 0.25-mm txheej ntawm chromatographic silica gel sib tov.
Test Solution: 10mg ib ml, hauv dej
Standard Solution- Npaj ib qho kev daws teeb meem ntawm USP Glutamine RS hauv dej uas muaj kev paub txog qhov concentration ntawm 0.05mg ib ml.
Daim ntawv thov Volume: 5μL
Tsim Cov Txheej Txheem Txheej Txheem: sib xyaw ntawm butyl cawv, dej, thiab glacial acetic acid (3: 1: 1).
Spray Reagent-Dissolve 0.2g ntawm ninhydrin hauv 100ml ntawm kev sib xyaw ntawm butyl cawv thiab 2 N acetic acid (95: 5)
Cov txheej txheem-Ua raws li qhia rau nyias-txheej chromatography nyob rau hauv Chromatography <621>, ces qhuav lub phaj ntawm 80 ℃ rau 30 feeb.Txau lub phaj nrog cov tshuaj tsuag reagent, cua sov ntawm 80 ℃ rau 10 feeb, thiab tshuaj xyuas hauv qab lub teeb dawb: tsis muaj qhov chaw thib ob hauv chromatogram tau los ntawm cov tshuaj ntsuam xyuas yog qhov loj dua lossis hnyav dua li qhov chaw tseem ceeb hauv chromatogram tau los ntawm cov tshuaj standrad. (0.5%)
Organic Volatile Impurities, Txoj Kev I <467>: Ua tau raws li qhov yuav tsum tau ua.
Asssy-Hloov txog 150mg ntawm Glutamine, raug hnyav, mus rau 125ml hwj, dissolbe hauv 3ml ntawm formic acid thiab 50ml ntawm glacial acetic acid, thiab titrate nrog 0.1 N perchloric acid VS txiav txim qhov kawg potentiometrically.Ua ib qho kev txiav txim siab dawb paug, thiab kho qhov tsim nyog (saib Titrimetry<541>).Txhua ml ntawm 0.1 N perchloric acid yog sib npaug rau 14.615 mg ntawm C5H10N2O3