Histamine Dihydrochloride CAS 56-92-8 Assay 98.5 ~ 101.0% (Titration) Factory

Histamine Dihydrochloride (CAS: 56-92-8) EP9.0 Hanyar Gwaji VolumeⅡ
BAYANI
Histamine dihydrochloride ya ƙunshi ba kasa da 98.5 bisa dari kuma bai wuce daidai da 101.0 bisa dari na 2- (1H-imidazol-4-yl)ethan-1-amine dihydrochloride, lissafta tare da magana da busasshen abu.
HALAYE
Farar fari ko kusan fari, crystalline foda ko lu'ulu'u marasa launi, hygroscopic, mai narkewa sosai cikin ruwa, mai narkewa cikin barasa.
GANO
Alamar farko: A, D.
Na biyu ganewa: B, C, D
A. Bincika ta infrared absorption spectrophotometry (2.2.24), kwatanta da bakan da aka samu tare da histamine dihydrochloride CRS.Bincika azaman fayafai da aka shirya ta amfani da 1 MG na abu.
B. Yi nazarin chromatograms da aka samu a gwajin don histidine.Babban tabo a cikin chromatogram da aka samu tare da maganin gwaji (b) yayi kama da matsayi, launi da girma zuwa babban tabo a cikin chromatogram da aka samu tare da bayani na tunani (a).
C. Narke 0.1 g a cikin 7 ml na ruwa R kuma ƙara 3 ml na 200 g / L bayani na sodium hydroxide R. Narke 50mg na sulfanilic acid R a cikin cakuda 0.1 mL na hydrochloric acid R da 10 ml na ruwa R kuma ƙara 0.1 ml na maganin sodium nitrite R. Ƙara bayani na biyu zuwa na farko da haɗuwa.Ana samar da launi ja.
D. Yana ba da amsa (a) na chlorides (2.3.1).
GWAJI
Magani S. Narkar da 0.5g a cikin ruwa-free carbon dioxide R shirya daga distilled ruwa R kuma tsarma zuwa 10 ml tare da sauran ƙarfi.
Bayyanar mafita.Magani S a bayyane yake (2.2.1) kuma bai fi tsananin launi ba fiye da maganin tunani Y7 (2.2.2, Hanyar II).
pH (2.2.3).Matsakaicin pH na S shine 2.85 zuwa 3.60.
Histidine.Bincika ta chromatography na bakin ciki-Layer (2.2.27), ta amfani da TLC silica gel G farantin R.
Maganin gwaji (a).Narkar da 0.5g na abun da za a bincika a cikin ruwa R kuma a tsoma zuwa 10 ml tare da sauran ƙarfi iri ɗaya.
Maganin gwaji (b).Tsarma 2 ml na maganin gwajin (a) zuwa 10 ml da ruwa R.
Maganin Magana (a).Narkar da 0.1 g na histamine dihydrochloride CRS a cikin ruwa R kuma a tsarma zuwa 10 ml tare da sauran ƙarfi iri ɗaya.
Maganin Magana (b).Narkar da 50 MG na histidine monohydrochloride R a cikin ruwa R kuma a tsarma zuwa 100 ml tare da sauran ƙarfi iri ɗaya.
Maganin Magana (c).Mix 1 ml na maganin gwaji (a) da 1 ml na maganin tunani (b).
Aiwatar da farantin 1 μL na maganin gwaji (a), 1 μL na maganin gwajin gwaji (b), 1 μL na bayani mai mahimmanci (a), 1 μL na bayani mai mahimmanci (b) da 2 μL na bayani (c).Haɓaka kan hanyar 15cm ta amfani da cakuda 5volumes na maida hankali ammonia R, 20 juzu'i na ruwa R da 75 na acetonitrile R. Busa farantin a halin yanzu na iska.Maimaita ci gaban a cikin wannan shugabanci, bushe farantin a cikin wani curren na iska da kuma fesa tare da ninhydrin bayani R1.Gasa farantin a 110 ° C na minti 10.Duk wani wuri da ya dace da histidine a cikin chromatogram da aka samu tare da maganin gwaji (a) bai fi ƙarfin tabo a cikin chromatogram da aka samu tare da bayani ba (b) (1%).Gwajin ba ta da inganci sai dai idan chromatogram da aka samu tare da bayani na tunani (c) ya nuna rarrabu 2 a sarari.
Sulfates (2.4.13).3ml na bayani S diluted zuwa 15 ml tare da distilled ruwa R ya bi iyakar gwajin sulfates (0.1%).
Asarar bushewa (2.2.32).Ba fiye da kashi 0.5 ba, ƙaddara akan 0.20 g ta bushewa a cikin tanda a 105 ° C.
Sulfated ash (2.4.14).Ba fiye da kashi 0.1 ba, an ƙaddara akan 0.5 g.
ASSAY
Narkar da 0.080 g a cikin cakuda 5.0 ml na 0.01 M hydrochloric acid da 50 ml na barasa R. Yi aikin titration mai ƙarfi (2.2.20), ta amfani da 0.1 M sodium hydroxide.Karanta ƙarar da aka ƙara tsakanin maki na farko da na uku na karkarwa.
1ml na 0.1 M sodium hydroxideis daidai da 9.203 MG na C5H11Cl2N3.
AJIYA
Ajiye a cikin akwati marar iska, kariya daga haske.