Intangiriro

Mubikorwa byo gukora imiti, ibishishwa bikoreshwa cyane mubice byinshi bya synthesis ya API, gukuramo, kweza no gutunganya. Ariko, niba iyi mashanyarazi kama idakuwe burundu kubicuruzwa byanyuma, "ibisigazwa bisigaye" bizashirwaho. Imiti imwe n'imwe ifite uburozi, kanseri cyangwa izindi ngaruka zishobora guteza ubuzima, bityo rero, kugenzura neza ibikubiye mu bisigazwa by’ibisigisigi muri farumasi ntabwo ari ihuriro ryingenzi ryo kurinda umutekano w’imiti y’abarwayi, ahubwo ni n’ingenzi mu micungire y’imiti y’imiti.

Mu isesengura ry'umutwe, icyitegererezo gifunzwe mu kintu cyihariye cyo gushyushya, kugirango ibice bihindagurika birekurwe mumwanya wa gaze hejuru ya kontineri, hanyuma iyi gaze yinjizwe muri chromatografi ya gaze kugirango isesengurwe. Kwizerwa nukuri kwintambwe isa nkiyoroshye biterwa ahanini nurufunguzo rukoreshwa - imitwe yumutwe.

Incamake yuburyo busigaye bwo gusesengura uburyo

Ubwoko butandukanye bwumuti usigaye ushobora kuboneka muri farumasi, hamwe nuburozi butandukanye bwuburozi, bigomba gushyirwa mubyiciro no gucungwa ukurikije ingaruka zishobora guterwa mugihe byasesenguwe kandi bikagenzurwa. Urungano mpuzamahanga rwasubiwemo ibyibutsa byibutsa gushyira ibisigazwa bisigaye mubyiciro bitatu bikurikira:

1. Icyiciro cya 1: Umuti wabujijwe

Harimo benzene, methylene chloride, 1,2-dichloroethane, karubone tetrachloride, nibindi, hamwe na kanseri ikomeye kandi byangiza ibidukikije, bigomba kwirindwa mugikorwa cyo kubyaza umusaruro. Imipaka igenzurwa cyane kandi mubisanzwe ibarwa kurwego rwa ppm cyangwa no munsi.

2. Icyiciro cya 2: Umuti ukurikiza igenzura rito

Harimo toluene, acetonitrile, DMF, inzoga ya isopropyl nibindi. Imyaka yibi bishishwa iremewe kurenza urugero, ariko iracyafite ingaruka zuburozi. Imipaka yashyizweho ishingiye kuri ADI kandi mubisanzwe bisaba gukurikiranwa gukomeye.

3. Icyiciro cya 3: Umuyoboro muke wuburozi

Muri byo harimo Ethanol, propanol, Ethyl acetate, n'ibindi, bifite uburozi buke ku bantu kandi muri rusange bifatwa nk'umutekano ku miti igera kuri buri munsi ya mg 50.

Kugirango tumenye neza ubwoko n'ibirimo biriya bisigazwa bisigaye, gazi chromatografiya (GC) nubu ni bwo buryo bukuru bwo gusesengura ibintu, bufite inyungu zikomeye zo kumva neza, gutandukana cyane, no gukoreshwa ku bintu bihindagurika, bishobora kuzuza ibisabwa kugira ngo hasesengurwe ibisigazwa bisigaye kugira ngo hamenyekane ibimenyetso.

Muburyo butandukanye bwo gutera inshinge za meteorologiya chromatografiya, tekinoroji yo gutera umutwe ikoreshwa cyane mugushakisha imiti isigaye muri farumasi. Ikoranabuhanga rinyuze mu rukundo rw'urwo rugero rufunze mu icupa ry'umutwe, rishyushye ku bushyuhe bukwiye, ni igisubizo mu cyitegererezo cyo guhindagurika mu mwanya wa gaze ya icupa, hanyuma kiva mu kirere kugira ngo gikuremo gaze ya gaze yatijwe muri GC kugira ngo isesengurwe.

Ibyiza byo kugaburira umutwe harimo:

• Kugabanya icyitegererezo mbere yo kuvurwa.
• Kunoza imyororokere no gutuza: mugucunga neza ubushyuhe bwubushyuhe nigihe, icyitegererezo gihindagurika kirahoraho, kugabanya amakosa yibikorwa;
• Irinde kwanduza cyangwa kwangiza inkingi: igice cya gaze gusa cyinjijwe muri sisitemu ya chromatografiya, igabanya cyane kwivanga kwibintu bidahindagurika hamwe ninkingi na detector.
• Birakwiye gusesengura byikora: sisitemu yo gutera inshinge irashobora guhuzwa na autosampler, ikwiranye nibisabwa byinshi byinjira.

Nyamara, icyitegererezo gihamye kandi cyizewe, icyuma cyumutwe, ni ntangarugero mu gusesengura neza kandi neza mu mutwe, ntabwo bigenga gusa imyitwarire ihindagurika n'ingaruka zifatika z'icyitegererezo, ariko kandi bigira ingaruka ku bisubizo by'isesengura rya nyuma.

Ibisobanuro n'ingaruka z'umutwe wumutwe

Muburyo bwo gutoranya umutwe, gushyushya no guhindagurika byintangarugero hamwe nuburyo bwo kubona umwanya wa gaze byombi bibera mumashanyarazi nko mu bikoresho byo mu kirere, nubwo bisa nkaho byoroshye, ariko igishushanyo mbonera n’imikorere y’ibikoresho byo mu mutwe bigira ingaruka zikomeye ku kwizerwa kwa gahunda zose zisesenguye.
Umwanya wibikoresho byumutwe ni urugero rwicyitegererezo cyagenewe gutera inshinge mumutwe wa gazi chromatografiya. Ubwubatsi busanzwe bugizwe nibice bikurikira:

Icupa: muri rusange bikozwe mu kirahure kinini cya borosilike, hamwe nubushyuhe bwo hejuru bwo guhangana nubushyuhe bwa chimique, bikunze kuboneka muri 10ml, 20ml, cyangwa ingano nini;

Gufungura icupa / urudodo: ahanini gufungura 20mm bisanzwe, bikwiranye na capit ya aluminium na sisitemu ya autosampling;

Cap: mubisanzwe ukanda mubintu byujuje ibisabwa kugirango umenye amacupa;

Igipapuro: hari PTFE hamwe na silicone yibigize ibikoresho, hamwe nubushyuhe bwiza bwo kurwanya ubushyuhe hamwe nubusembure bwa chimique, birashobora kwihanganira ibyitegererezo byinshi bitarinze kumeneka.

Uruhare runini rwicupa ryumutwe ni ugutanga ibidukikije bifunze, bitagira ingano kandi bigenzurwa, ni imashanyarazi ihindagurika murugero mugihe cyubushyuhe nuburyo buryo yewe icupa riri hejuru yumwanya wa gaze, gushiraho gazi iringaniza ya gazi ihagarariwe na solvent yibitekerezo byumwimerere.

By'umwihariko, uruhare rwayo rugaragarira mu ngingo zikurikira:

Ingwate: gufunga neza kugirango umenye neza ko icyitegererezo muburyo bwo gushyushya cyangwa kuruhuka buri gihe bitazaterwa no gutemba no gutakaza ibishishwa;

Shyiramo ibikoresho.

Imiterere ihoraho: amacupa asanzwe agira uruhare mumitwe yumutekano no kubyara, byorohereza kugereranya no kugereranya ibisubizo byisesenguye.

Umwanya wibikoresho bya pessimistic antipathie ikoreshwa kumashanyarazi yikora. Urujya n'uruza rw'akazi ni ubu bukurikira:

1. Igisubizo cyicyitegererezo cyongewe kumutwe wumutwe kandi gifunze;
2. Autosampler igaburira vial muburyo bwo gushyushya ubushyuhe;
3. Icyitegererezo gishyushye muri vial kugeza ubushyuhe bwashyizweho kandi ni ibice bihindagurika byimukira mumutwe;
4. Urushinge rwo gutera inshinge rutobora gasike kandi rukuramo gaze ya gaze mumutwe;
5. Gazi igaburirwa muri chromatografi ya gaz kugirango itandukane kandi itahure.

Muri ubu buryo, ituze ryimiterere, imikorere ya gasketi, hamwe no gufunga ibyuma byumutwe bifitanye isano itaziguye no guhitamo icyitegererezo hamwe nukuri kwicyitegererezo. By'umwihariko, ikoreshwa ryibikoresho bisanzwe, byizewe byumutwe mubikorwa byikora ni urufunguzo rwo kwemeza ko inzira yisesengura ikora neza kandi igabanya ibipimo byatsinzwe.

Ni ukubera iki Ibikoresho byo mu mutwe ari ngombwa?

Nubwo gazi chromatografi na detector aribikoresho byibanze mu gusesengura ibisigisigi bisigaye, uruhare rwikibanza cyumutwe ni ingenzi cyane. Nkumutwara wa analyite kuva icyitegererezo cyo gutera inshinge, imikorere yacyo ifitanye isano itaziguye na sisitemu yo gusesengura yose hamwe no kwizerwa kwamakuru.

1. Icyitegererezo cy'ubunyangamugayo no kugenzura ihindagurika

Umuti usigara usanga ahanini utetse cyane, ibinyabuzima bihindagurika cyane bishobora guhomba cyane mugihe cyo guhura, gushyushya cyangwa kubika. Niba imitwe yumutwe idashobora kubikwa mukidodo gikurikiranye mugihe cyisesengura, ibishobora guhinduka birashobora guhinduka, bikavamo ibisubizo bibogamye.

Ibikoresho byo mu rwego rwo hejuru birashobora gushyuha hejuru ya 100-150 ° C mugihe gifunze, byemeza ko ibice bihindagurika birekurwa kandi bigasesengurwa mugihe cyagenwe;

Kugenzura neza icyitegererezo kugirango ugere kuri gazi-yamazi iringaniye mubushyuhe burigihe nubunini byerekana neza ukuri no kubyara ibisubizo.

2. Ingaruka zo gufunga imikorere kubisubizo byisesenguye

Sisitemu yo gufunga umuyonga wa Headspace mubusanzwe igizwe nibice bitatu: ingofero, gaseke hamwe numunwa. Ikidodo kibi ahantu hose gishobora kuvamo icyitegererezo, urusaku rwinshi rwinshi, cyangwa se icyitegererezo cyanduye.

Igipimo cyiza cya PTFE / silicone ntishobora kwihanganira ubushyuhe bwinshi n’imiti gusa, ariko kandi irashobora kwihanganira imyobo myinshi kandi ikagumana kashe nziza;

Igipimo cyiza cya glande cyangwa glande irekuye irashobora gutuma umusemburo uhunga mbere yisesengura cyangwa mugihe cyo gushyushya, bigira ingaruka kumpinga no kugabanya ubwinshi bwumubare.

3. Guhuza na sisitemu ya autosampling

Gutera inshinge zo mu mutwe zikoreshwa cyane muri laboratoire zigezweho kugirango tunoze imikorere kandi ihamye y'ibisubizo, kandi igishushanyo mbonera cya Headspace vial ituma ishobora guhuzwa neza na marike akomeye ya sisitemu yo gutera inshinge.

Ibipimo bisanzwe byemeza ko amacupa ashobora guhita amenyekana, neza neza kandi agacumita muri inshinge;

Kugabanya amakosa yintoki bitezimbere icyitegererezo cyo gutunganya no guhuza amakuru, bigatuma Headspace vial nziza cyane kubintu byinshi byinjira.

4. Kutagira imiti yibikoresho

Ubuhanga bwa chimie yamacupa nibikoresho bifunga kashe ntibigomba kwirengagizwa mugihe dusesenguye ibishashara. Ibikoresho bitujuje ubuziranenge birashobora kwamamaza cyangwa kubyitwaramo na molekile zishonga, biganisha kubisubizo bibogamye.

Ikirahuri cya Borosilike kirimo imiti kandi ihagaze neza, irinda ibishishwa byangirika cyangwa kwangirika kwubushyuhe;

Kuri sisitemu zidasanzwe zidasanzwe, gasketi ikozwe mubikoresho byihariye irasabwa kugirango hamenyekane ibyiyumvo byerekana kandi bihamye.

Umuyoboro wa Headspace nturenze gusa icyitegererezo cyoroshye, ni ikintu cyingenzi mugukora ibishoboka byose kugirango ibisubizo byisesengura bisigara ari ukuri, bihamye kandi byororoka. Ifata imirimo myinshi yingenzi murwego rwose rwisesengura, nko kurinda kashe, kugenzura ihindagurika, guhuza sisitemu, garanti yimiti idahwitse, nibindi.

Ibintu by'ingenzi muguhitamo Umwanya Ukwiye Umwanya

Isesengura ryibisigisigi bisigaye, guhitamo icyerekezo gikwiye cyumutwe nikintu gisabwa kugirango tumenye neza amakuru hamwe nuburyo buhoraho. Ibikenerwa bitandukanye mubigeragezo, ubwoko bwikitegererezo hamwe nibikoresho bya platform bifite ibisabwa bitandukanye kumutwe wibikoresho byumutwe, imiterere nibikorwa. Ibintu byingenzi bikurikira bigomba kwitabwaho muguhitamo ikibanza cyumutwe:

1. Ibikoresho: ubwoko bwikirahure no gukorera mu mucyo

• Icyiciro cya I borosilicate ikirahure: icupa ryatoranijwe ryibikoresho byo gusesengura bisigaye. Ubushuhe buhebuje hamwe nubushakashatsi bwimiti hamwe nubushyuhe buke cyane bwa ion yaguye birinda imiti yimiti hagati yumuti n icupa, ikirinda ibyiza cyangwa kutabangamira ibimenyetso.
• Ubucucike bukabije bw'icupa: yemerera kwitegereza byihuse icyitegererezo mugihe cyo gutera, kugenzura cyangwa kugenzura ubuziranenge, nko kuba hari imvura igwa, umubare nyawo wamazi, nibindi, kimwe no kumenyekana byoroshye na sisitemu zikoresha.

2. Guhitamo amajwi: bikunze gukoreshwa 10ml, 20ml

Guhitamo ubushobozi bwa Headspace vial ubushobozi bigomba gushingira kumahuriro yibintu bikurikira:

• Ingano y'icyitegererezo: Mubisanzwe ingano yicyitegererezo igera kuri 50% yubunini bwamacupa kugirango harebwe umwanya uhagije (agace ka gaze) kuburinganire bwa volatilisation;
• Uburyo Bwisesengura Ibisabwa: Kurugero, USP <467> uburyo busigaye bwo gukemura ibibazo birasaba gukoresha vial ya 20 ml yumutwe;
• Guhuza Autosampler: wemeze ko icupa ryatoranijwe rishyigikira igikoresho cyakoreshejwe, cyane cyane icupa hejuru ya aperture.

3. Gupfuka ubwoko bwa gasike: gufunga no guhuza imiti

Ibikoresho. kumashanyarazi akomeye cyangwa yangiza, urashobora guhitamo igipimo cyiza-cyiza cya PTFE gati ishimangirwa.

Ubwoko bw'icupa: Ibipapuro bya aluminiyumu bikwiranye nibikoresho byinshi, hamwe na glande ifatanye kandi bifunze neza; Imashini ya magnetique ikwiranye na sisitemu yo gukoresha autosampling hamwe na magnetique iranga, ifasha kunoza uburyo bwo kugaburira no kugena neza; Ingofero zifunitse, nubwo byoroshye kubikorwa byintoki, ntibishobora gufunga kimwe nubwoko bwa gland kandi birakwiriye mubyiciro byiterambere cyangwa bitari byinshi-byinjira.

4. Kongera gukoreshwa no gutekereza kubiciro

Ibirahuri byongeye gukoreshwa (bisaba koza ubushyuhe bwo hejuru no kuboneza urubyaro) birakwiriye muburyo bumwe butari imiti cyangwa ubushakashatsi bwiterambere kandi burashobora kugabanya ibiciro byigihe kirekire;

Nyamara, kubikorwa bya GMP cyangwa laboratoire igenzura ubuziranenge, inkono imwe ikoreshwa nibyiza mugukora isuku no kwirinda kwanduzanya;

Mugihe ugura mubice, ni ngombwa kandi gupima ubuziranenge bwibicuruzwa, icyiciro kimwe kugeza ku cyiciro, hamwe nigiciro cyo guhitamo utanga isoko itanga impirimbanyi yimikorere nigiciro.

Guhitamo gushyira mu gaciro vial headace ntabwo ari ibikorwa byibanze gusa, ahubwo ni nuburyo bwo kugenzura ubuziranenge. Guhitamo ibintu byose bisa nkibito bifite uruhare runini mubisubizo byukuri, sisitemu ihamye hamwe na laboratoire. Kubwibyo, gusobanukirwa byimbitse kubintu byingenzi nubushobozi bwumwuga kuri buri mutekinisiye ukora mu isesengura ryimiti.

Ibibazo Bikunze Kubazwa

Nubwo ibirahuri byumutwe bikoreshwa cyane mubisesengura bisigaye, urukurikirane rwibibazo rushobora kuvuka mubikorwa kubera gufata nabi cyangwa guhitamo ibikoreshwa. Ibikurikira nibibazo bisanzwe hamwe nibyifuzo byo gukumira:

1. Nigute twakwirinda icyitegererezo cyanduye

Kwanduzanya kwanduza ntabwo bigira ingaruka gusa ku bisubizo by’isesengura, ahubwo birashobora no gutera igihe kirekire kwihisha hamwe na sisitemu yo gutahura, cyane cyane ku kaga gakomeye iyo usesenguye urwego rwo hasi. Ingamba zikurikira zirashobora gukemura neza iki kibazo:

• Shyira imbere ikoreshwa ryibikoresho bikoreshwa hamwe na cap pad: ubu ni bwo buryo butaziguye kandi bunoze, cyane cyane mu kugenzura ubuziranenge bwa farumasi no gupima amabwiriza;
• Simbuza cyangwa usukure neza ibibindi byakoreshejwe.
• Uburyo bukomeye bwo gutanga: koresha ibikoresho byabugenewe kugirango wirinde icyitegererezo gitonyanga kumacupa;
• Isuku yintebe yintebe hejuru na gants: mugihe utunganya ibishishwa bihindagurika, gants zigomba guhinduka buri gihe kugirango wirinde kwanduza kwanduza.

2. Kumeneka kumutwe mugihe cyo gushyushya

Mu isesengura ryumutwe, icyitegererezo kigomba gushyuha kugeza kuri 80-120 ° C cyangwa hejuru. Niba imipira cyangwa gasketi bidafunze neza, ibishishwa birashobora guhunga mugihe cyo gushyushya, bikavamo guhindagurika kwamakuru cyangwa ibisubizo bike.

• Hitamo gasketi nziza: bagomba kugira ubushyuhe bwiza no guhindagurika kugirango barebe ko kashe idacogora;
• Gukosora imbaraga zo gufata: gufata intoki cyangwa mu buryo bwikora bigomba kuba bitagereranywa, kurekura birashobora gutemba, gukomera birashobora gusenya gasike cyangwa bigatuma icupa riturika;
• Kugenzura buri gihe urushinge rwa sisitemu yo kugaburira: urushinge rwambarwa cyangwa rwahinduwe rushobora kubuza gaze kwifunga, bikavamo kumeneka;
• Gushiraho ubushyuhe bushyize mu gaciro: ntigomba kurenza urugero rwo hejuru rwubushyuhe bwa gaze cyangwa cap, mubisanzwe bigenzurwa murwego rwa 110-130 ℃ ni umutekano.

3. Ibyifuzo byo gusukura no kubika ibyifuzo

Kubikoresha byongeye gukoreshwa bishobora kugira uruhare mukugenzura ibiciro cyangwa icyiciro cyiterambere ryiterambere, hagomba kwitabwaho cyane kubikorwa byogusukura no kubika kugirango hirindwe kwanduza umwanda cyangwa ibisigazwa bisigaye:

• Igitekerezo cyo gusukura intambwe: kwoza inshuro nyinshi n'amazi ya deionion; kwoza hamwe n'umuti ukwiye; isuku ya ultrasonic bitewe nurwego rwanduye; ubushyuhe bwo hejuru bwumutse kuri 105 ℃ -120 ℃ kugirango harebwe niba ntamazi asigara cyangwa umusemburo.
• Ibyifuzo byo kubika: isuku, yumye kandi ifunze, kugirango wirinde umukungugu, ibintu bihindagurika byongera kwanduza; mbere yo gukoresha niba ibitswe igihe kirekire, birasabwa kongera kugenzura no kongera gukora isuku; irinde kumara igihe kinini urumuri rwizuba cyangwa ubushyuhe bwinshi, kugirango wirinde kwangirika kwikirahure cyangwa gasike.

Ukoresheje neza amakuru yingenzi yibikorwa, ntushobora gusa kunoza ukuri no gusubiramo ikizamini, ariko kandi ushobora kongera igihe cyumurimo wibikoresho no kugabanya igipimo cyatsinzwe. Kubintu byisesengura nkibisigisigi bisigaye, byunvikana cyane kubitandukanya, imiyoborere irambuye ya buri murongo wibikorwa ntigomba kwirengagizwa.

Umwanzuro

Muburyo bugenzurwa cyane kandi busobanutse bwisesengura ryibisigisigi bya farumasi, ikibanza cyumutwe, nubwo ari gito, gifite uruhare rukomeye kandi rukomeye. Kuva mububiko, gufunga no gushyushya icyitegererezo, kugeza guhuza na sisitemu ya autosampling, niwo murongo wambere wo kwirwanaho murwego rwose rwisesengura kugirango hamenyekane neza amakuru.

Umwanya mwiza wumutwe ntushobora kurinda gusa ubusugire bwikitegererezo, gukumira igihombo cy’imihindagurikire, no kunoza uburyo bwo gutera inshinge, ariko kandi ni umusingi wa ngombwa wo kubyara cyane kandi byoroshye gutahura mu isesengura ryikora. Cyane cyane mugihe uhanganye nisesengura ryurwego rusabwa rusabwa nubuziranenge bwa farumasi, inenge ntoya, ibikoresho bidakwiye, cyangwa nigikorwa cyo kuzuza icyitegererezo kidafite ishingiro bizagira ingaruka zitari nke kubisubizo byisesengura.

Mugihe iterambere ryibiyobyabwenge no kugenzura ubuziranenge bikomeje kwiyongera kurwego rwo gutangiza no gutahura ibicuruzwa, ibipimo byubuziranenge bwibikoresho byo mumutwe nabyo birazamurwa. Uhereye kubintu byera, guhuza izina kugeza kuri sisitemu ihujwe, imiyoboro yumwanya wigihe kizaza ntigomba kuba ihamye kandi yizewe gusa, ahubwo igomba no kugira uruhare rwa "interineti isanzwe" muri laboratoire itegura igenamigambi, ifasha gukurikirana amakuru, kubyara uburyo no kuzamura igenzura ryiza.