I-D-Leucine CAS 328-38-1 HD-Leu-OH Assay 98.5~101.5% Ifektri Ikhwalithi ephezulu

pH
Thatha u-0.50g walo mkhiqizo, engeza u-50ml wamanzi, ukushisa ukuze uncibilike, uphole, futhi unqume ngokomthetho (Okujwayelekile 0631), inani le-pH kufanele libe ngu-5.5~6.5.
Ukudluliswa Kwesixazululo
Thatha u-0.50g walo mkhiqizo, engeza u-50ml wamanzi, ukushisa ukuncibilika, okupholile, i-ultraviolet-visible spectrophotometry (Umthetho ojwayelekile 0401), ulinganise ukudlulisa ku-430nm wavelength, hhayi ngaphansi kuka-98.0%.
I-Chloride
Thatha u-0.25g walo mkhiqizo futhi uwuhlole ngokomthetho (Umthetho ojwayelekile 0801).Uma kuqhathaniswa nesisombululo sokulawula esenziwe nge-5.0 ml yesisombululo esijwayelekile se-sodium chloride, akufanele sigxile kakhulu (0.02%).
I-sulfate
Thatha u-1.0g walo mkhiqizo futhi uwuhlole ngokomthetho (Umthetho ojwayelekile 0802).Uma kuqhathaniswa nesisombululo sokulawula esenziwe nge-2.0 ml yesisombululo esijwayelekile se-potassium sulfate, akufanele sigxile kakhulu (0.02%).
Usawoti we-ammonium
Thatha lo mkhiqizo ongu-0.10g, hlola ngokomthetho (Umthetho ojwayelekile 0808), bese uqhathanisa nesisombululo sokulawula esenziwe ngesisombululo se-ammonium chloride esijwayelekile esingu-2.0 ML, esingajulile (0.02%).
Amanye ama-Amino Acid
Thatha inani elifanele lalo mkhiqizo, engeza amanzi ukuze uncibilike futhi uhlambulule ukuze wenze isisombululo esiqukethe cishe u-20mg nge-lml ngayinye njengesixazululo sokuhlola;Thatha i-1ml yesilinganiso esinembile bese uyibeka ku-flask yokulinganisa engu-200ml, hlambulula esikalini ngamanzi, unyakazise, ​​njengesixazululo sokulawula;Thatha inani elifanele lereferensi ye-leucine kanye nereferensi ye-valine, futhi uyibeke kuflask yokulinganisa efanayo, amanzi ayengezwa ukuze ancibilike futhi ahlanjululwe ukuze kulungiswe isixazululo esiqukethe cishe u-0.4mg ngayinye ku-1ml njengesixazululo esifanelekile sohlelo.Ngokokuhlolwa kongqimba oluncane lwe-chromatography (Okujwayelekile 0502), donsa izixazululo ezintathu ezingenhla ngasinye ngo-5 u1, ngokulandelana, ku-silica gel G yepuleti lengqimba elincanyana, eline-acetic acid engu-n-butanol-water-glacial (3:1:1) ukuze kuthuthukiswe, ngemva kokuthunyelwa, ukomiswa komoya, ukufafaza nge-ninhydrin kusisombululo se-acetone (1-50), ukushisisa ngo-80°C kuze kuvele amabala, futhi kuhlolwe ngokushesha.Isixazululo sokulawula kufanele sibonise indawo ecacile, futhi isisombululo esisebenzayo sesistimu kufanele sibonise izindawo ezimbili ezihlukene ngokuphelele.Uma isisombululo sokuhlola sibonisa izindawo zokungcola, umbala akufanele ujule (0.5%) kunendawo eyinhloko yesisombululo sokulawula.
Ukulahlekelwa Ekumisweni
Thatha lo mkhiqizo, wome ku-105℃ amahora angu-3, ​​ukulahlekelwa isisindo akufanele kudlule u-0.2% (Umthetho ojwayelekile 0831).
Izinsalela ekushiseni
Thatha u-1.0g walo mkhiqizo futhi uwuhlole ngokomthetho (Umthetho ojwayelekile 0841).Okusele akumele kudlule u-0.1%.
Usawoti Wensimbi
Thatha u-1.5g walo mkhiqizo futhi uwuhlole ngokomthetho (Umthetho ojwayelekile 0807).Uma kuqhathaniswa nesixazululo sokulawula esenziwe nge-0.001% yesisombululo sensimbi esijwayelekile, ngeke sijule ().
Izinsimbi Ezisindayo
Izinsalela ezishiywe ngaphansi kwento yokuthatha insalela yokubasa ngeke ziqukathe izingxenye ezingaphezu kweziyi-10 esigidini sensimbi esindayo lapho ihlolwa ngokomthetho (Izimiso Ezijwayelekile 0821, Law II).
I-Arsenic Usawoti
Faka amanzi angu-5ml, u-1ml we-sulfuric acid no-10ml sulfurous acid, ukushisa kuvolumu engaba ngu-2ml emanzini okugeza, engeza amanzi angu-5ml, engeza isixazululo se-Drophise ammonia kuze kube yilapho inkomba ye-phenolphthalein ingathathi hlangothi, engeza i-hydrochloric acid 5ml, engeza amanzi ukwenza u-28ml. , ngokuvumelana nokuhlolwa komthetho (Izimiso Ezijwayelekile 0822 Umthetho wokuqala), kufanele uhambisane nezinhlinzeko (0.0001%).
I-Endotoxin yebhaktheriya
Thatha lo mkhiqizo, hlola ngokomthetho (Okujwayelekile 1143), i-lg leucine ngayinye equkethe i-endotoxin kufanele ibe ngaphansi kwama-25EU.(Okomjovo)
328-38-1 - Ukunqunywa kokuqukethwe
Thatha lo mkhiqizo cishe u-0.1g, isisindo esinembile, engeza i-anhydrous formic acid engu-1 ml encibilikisiwe, engeza i-glacial acetic acid engu-25ml, ngokuya ngendlela ye-potentiometric titration (Umthetho ojwayelekile 0701), ne-perchloric acid titration solution (O. 1 mol/L) titration , futhi imiphumela ye-titration yalungiswa ngokuhlolwa okungenalutho.I-1 ml ngayinye yesisombululo se-perchloric acid titration (0.1 mol/L) ihambisana no-13.12 mg we-C6H13N02.