L-Tryptophan CAS 73-22-3 (H-Trp-OH) Kev Ntsuam Xyuas 98.5 ~ 101.5% Lub Hoobkas Zoo

L-Tryptophan (H-Trp-OH) (CAS: 73-22-3) AJI 97 Test Method
Kev txheeb xyuas: Sib piv cov infrared absorption spectrum ntawm cov qauv nrog cov qauv ntawm cov txheej txheem potassium bromide disc.
Kev sib hloov tshwj xeeb [α]20 / D: Cov Qauv Qhuav, C = 1, H2O yaj los ntawm kev ua kom sov
Kev daws teeb meem (Kev xa tawm): 0.5g hauv 20ml ntawm 2 mol / L HCl, spectrophotometer, 430nm, 10mm cell thickness.
Chloride (Cl): 0.7g, A-1, ref: 0.40ml ntawm 0.01mol / L HCl
Ammonium (NH4): B-2
Sulfate (SO4): 1.2g, (1), ref: 0.50ml ntawm 0.005mol / L H2SO4
Hlau (Fe): 0.75g, (2), ref: 1.5ml ntawm Hlau Std.(0.01 mg/ml)
Heavy Metals (Pb): 2.0g, (4), ref: 2.0ml ntawm Pb Std.(0.01 mg/ml)
Arsenic (As2O3): 2.0g, (1), ref: 2.0ml ntawm As2O3 Std.
Lwm yam Amino Acids: H2O, Dissolve los ntawm sov (40 ℃) Test Sample: 50μg, A-6-a, tswj: L-Trp 0.25μg
Poob rau ziab: ntawm 105 ℃ rau 3 teev.
Residue ntawm Ignition (Sulfated): AJI Test 13
Assay: Cov qauv qhuav, 200mg, (1), 3ml ntawm formic acid, 50ml ntawm glacial acetic acid, 0.1mol/L HCLO4 1ml = 20.423mg C11H12N2O2
pH Test: 1.0g hauv 100ml ntawm H2O

L-Tryptophan (H-Trp-OH) (CAS: 73-22-3) USP35 Test Method
DEFINITION
Tryptophan muaj NLT 98.5% thiab NMT 101.5% ntawm C11H12N2O2, raws li L-Tryptophan, xam ntawm lub hauv paus qhuav.
IDENTIFICATION
A. INFRARED ABSORPTION <197K>
QHIA
txheej txheem
Piv txwv li: Muab 200 mg ntawm tryptophan rau hauv 125-mL hwj.Dissolve nyob rau hauv ib tug sib tov ntawm 3 mL ntawm formic acid thiab 50 mL ntawm glacial acetic acid.
Kev Ntsuas: Titrate nrog 0.1 N perchloric acid VS, txiav txim siab qhov kawg ntawm 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 20.42 mg ntawm C11H12N2O2.
Kev lees txais: 98.5% ~ 101.5% ntawm lub hauv paus qhuav
IMPURITIES
Inorganic impurities
RESIDUEON IGNITION <281>: NMT 0.1%
CHLORIDE THIAB SULFATE, Chloride <221>: Ib feem 0.73-g qhia tias tsis muaj cov tshuaj chloride ntau dua li 0.50 mL ntawm 0.020 N hydrochloric acid (0.05%).[CEEB TOOM- Maj mam ua kom sov cov qauv npaj kom yaj, yog tias tsim nyog.]
CHLORIDE THIAB SULFATE, Sulfate <221>: Ib feem 0.33-g qhia tias tsis muaj sulfate ntau dua li 0.10 mL ntawm 0.020 N sulfuric acid (0.03%).[CEEB TOOM- Maj mam ua kom sov cov qauv npaj kom yaj, yog tias tsim nyog.
Hlau <241>: NMT 30ppm
HEAVY METALS, Method II <231>: NMT 15ppm
Organic impurities
PROCEDURE 1
Kev daws A: Trifluoroacetic acid hauv dej (1 mL / L)
Kev daws B: Trifluoroacetic acid hauv acetonitrile thiab dej tov (80:20) (1 mL / L trifluoroacetic acid tov)
Kev daws teeb meem: 1.0 mg / L txhua ntawm USP Tryptophan Related Compound A RS thiab USP Tryptophan Related Compound B RS hauv dej
Piv txwv li: 10.0 mg / mL ntawm tryptophan hauv dej
Kev daws teeb meem tsim nyog: 1.0 mg / L ntawm USP Tryptophan Related Compound B RS hauv dej
Mobile theem: Saib lub gradient table hauv qab no.

Chromatographic system (Saib Chromatography <621>, System Suitability.)
Qauv: LC
Detector: UV 220 nm
Kem: 4.6-mm × 25-cm;5-µm ntim L1
Kem kub: 30 °
Tus nqi ntws: 1 mL / min
Kev txhaj tshuaj loj: 20 µL
Qhov system haum
Qauv: Kev daws teeb meem tsim nyog
Suitability xav tau
Tus txheeb ze tus qauv sib txawv: NMT 5.0%
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Txheeb xyuas qhov feem pua ​​​​ntawm txhua qhov tsis muaj qhov tsis huv hauv feem ntawm Tryptophan coj mus rau:
Result = (rU/rS) × (CS/CU) × 100
rU = thaj chaw ncov ntawm txhua qhov tsis muaj kev txwv tsis pub muaj nyob rau hauv cov qauv tshuaj
rS = thaj chaw ncov ntawm tryptophan muaj feem xyuam nrog B hauv cov txheej txheem kev daws teeb meem
CS = concentration ntawm USP Tryptophan Related Compound B RS nyob rau hauv tus qauv tov (µg/mL)
CU = concentration ntawm tryptophan nyob rau hauv cov qauv tov (µg/mL)
Kev lees txais
Tag nrho cov impurities 1: NMT 0.01% ntawm tag nrho cov impurities eluting ua ntej lub tryptophan ncov
Tag nrho cov impurities 2: NMT 0.03% ntawm tag nrho cov impurities eluting tom qab tryptophan ncov.[CEEB TOOM-Tshem tawm lub ncov rau tryptophan ntsig txog compound B.]
Tryptophan ntsig txog compound A: Yog tias qhov siab tshaj plaws rau tryptophan ntsig txog compound A tau pom nyob rau hauv cov qauv kev daws teeb meem, tom qab ntawd ua qhov kev sim rau txheej txheem 2: txwv ntawm Tryptophan Related Compound A, hauv qab no.
LUS CEEB TOOM 2: LIMIT NTAWM TRYPTOPHAN RELATED COMPOUND A
Tshuaj A: 18 mM monobasic sodium phosphate, lim thiab degassed (pH 2.5), thiab acetonitrile (9: 1)
Tshuaj B: 10 mM monobasic sodium phosphate, lim thiab degassed (pH 2.5), thiab acetonitrile (1: 1)
Kev daws C: Acetonitrile hauv dej (7: 3)
Kev daws teeb meem: 0.1 mg / L ntawm USP Tryptophan Related Compound A RS hauv dej
Piv txwv li: 10.0 mg / mL ntawm tryptophan hauv dej
Mobile theem: Saib lub gradient table hauv qab no

Chromatographic system
(Saib Chromatography <621>, System Suitability.)
Qauv: LC
Detector: UV 216 nm
Kem: 3.9-mm × 15-cm;5-µm ntim L1
Kem kub: 30 °
Tus nqi ntws: 1 mL / min
Kev txhaj tshuaj loj: 20 µL
Qhov system haum
Qauv: Standard tov
Suitability xav tau
Tus txheeb ze tus qauv sib txawv: NMT 5.0%
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Xam qhov feem pua ​​​​ntawm tryptophan muaj feem xyuam nrog
Ib feem ntawm Tryptophan noj:
Result = (rU/rS) × (CS/CU) × 100
rU = thaj tsam ncov ntawm tryptophan muaj feem xyuam nrog A hauv cov qauv tshuaj
rS = thaj chaw ncov ntawm tryptophan muaj feem xyuam nrog cov ntsiab lus A hauv Standard tov
CS = concentration ntawm USP Tryptophan Related Compound A RS nyob rau hauv Standard tov (µg/mL)
CU = concentration ntawm tryptophan nyob rau hauv cov qauv tov (µg/mL)
Kev lees txais: NMT 10 ppm
TSEEM CEEB
OPTICAL ROOTATION, Kev sib hloov tshwj xeeb <781S>: -29.4 ° txog -32.8 °
Piv txwv li: 10 mg / mL, hauv dej.[CEEB TOOM-Kub maj mam yaj, yog tias tsim nyog.]
PH <791>: 5.5 ~ 7.0, hauv kev daws (1 hauv 100)
LOSS ON DRYING <731>: Qhuav ib qho qauv ntawm 105 ° rau 3 h: nws poob NMT 0.3% ntawm nws qhov hnyav.
TSEEM CEEB
PACKAGING THIAB STORAGE: Khaws rau hauv cov thawv kaw kom zoo
USP REFERENCE STANDARDS <11>
USP L-Tryptophan RS
USP Tryptophan Related Compound A RS
3,3′-[Ethylidenebis(1H-indole-1,3-diyl)]bis[2S)-2-aminopropanoic] acid.C24H26N4O4 432.49
USP Tryptophan Related Compound B RS
2-Acetamido-3-(1H-indol-3-yl)propanoic acid.C13H14N2O3 246.3