Isingeniso

Enqubweni yokukhiqiza imithi, izinyibilikisi zisetshenziswa kabanzi ezicini eziningi zokwenziwa kwe-API, ukukhishwa, ukuhlanza kanye nezinqubo zokwakheka. Kodwa-ke, uma lezi zinyibilikisi eziphilayo zingasuswa ngokuphelele kumkhiqizo wokugcina, kuzokwakhiwa “izinyibilikisi ezisele”. Ezinye izinyibilikisi zinobuthi, umdlavuza noma ezinye izingozi zempilo ezingaba khona, ngakho-ke, ukulawula okuqinile kokuqukethwe kwezinyibilikisi ezisele emithini yemithi akuyona nje isixhumanisi esibalulekile sokuqinisekisa ukuphepha kwemithi yeziguli, kodwa futhi kuyisici esibalulekile sokuphathwa kwekhwalithi yemithi.

Ekuhlaziyweni kwesikhala sekhanda, isampula ivalwa esitsheni esithile sokushisa, ukuze izingxenye eziguquguqukayo zikhishwe esikhaleni segesi esingaphezu kwesitsha, bese le gesi ifakwa ku-chromatograph yegesi ukuze ihlaziywe. Ukuthembeka nokunemba kwalesi sinyathelo esibonakala silula kuncike kakhulu ezintweni ezibalulekile ezisetshenziswayo - ama-headspace vials.

Ukubuka Konke Kwezindlela Zokuhlaziya I-Residual Solvent

Izinhlobonhlobo eziningi zezinyibilikisi ezisele ezingaba khona emithini yemithi, ezinezakhiwo ezinobuthi ezahlukene, zidinga ukuhlukaniswa ngezigaba futhi ziphathwe ngokwezingozi zazo ezingaba khona lapho zihlaziywa futhi zilawulwa. Izikhumbuzo zokuhlukaniswa ezibuyekezwa ontanga zomhlaba wonke zihlukanisa izinyibilikisi ezisele ngezigaba ezintathu ezilandelayo:

1. Isigaba 1: Izinyibilikisi ezingavunyelwe

Kufaka phakathi i-benzene, i-methylene chloride, i-1,2-dichloroethane, i-carbon tetrachloride, njll., enobungozi obukhulu bomdlavuza kanye nezingozi zemvelo, kufanele kugwenywe enqubweni yokukhiqiza. Imikhawulo ilawulwa kakhulu futhi ivame ukubalwa emazingeni e-ppm noma ngisho nangaphansi.

2. Isigaba 2: Izinyibilikisi zilawulwa ngokulinganiselwe

Kufaka phakathi i-toluene, i-acetonitrile, i-DMF, i-isopropyl alcohol njalo njalo. Ubudala balezi zinyibilikisi buyamukeleka ngaphansi kwemingcele ethile, kodwa zisenezingozi ezithile zobuthi. Imingcele ibekwa ngokusekelwe ku-ADI futhi ngokuvamile idinga ukuqapha okuqinile.

3. Isigaba 3: Izithako ezinciphile ezinobuthi

Lokhu kufaka phakathi i-ethanol, i-propanol, i-ethyl acetate, njll., ezinobuthi obuphansi kubantu futhi ngokuvamile zibhekwa njengeziphephile emithini kuze kufike ekuthathweni kwansuku zonke okungu-50 mg.

Ukuze kutholakale ngokunembile uhlobo nokuqukethwe kwalezi zinyibilikisi ezisele, i-gas chromatography (GC) njengamanje iyindlela yokuhlaziya esetshenziswa kakhulu, enezinzuzo ezibalulekile zokuzwela okuphezulu, ukusebenza kahle kokuhlukanisa okuphezulu, kanye nokusebenza kuma-volatile compounds, angahlangabezana nezidingo zokuhlaziywa kwe-residual solvent ukuze kutholakale umkhondo.

Phakathi kwezindlela ezahlukene zokujova ze-chromatography yesimo sezulu, ubuchwepheshe bokujova i-headspace busetshenziswa kabanzi ekutholeni izinyibilikisi ezisele emithini yemithi. Ubuchwepheshe ngokusebenzisa uthando lwaleso sampula esivalwe ebhodleleni le-headspace, elifudunyezwa ekushiseni okufanele, yi-solvent ekuguqukeni kwesampula iye esikhaleni segesi yebhodlela, bese ikhishwa esikhaleni ukuze kukhishwe umthamo othile wegesi oqashiwe ku-GC ukuze uhlaziywe.

Izinzuzo zokudla okune-headspace zifaka:

• Ukwelashwa kwesampula okuncishisiwe ngaphambi kokwelashwa: akukho ukukhishwa kwe-solvent okuyinkimbinkimbi noma imisebenzi yokuxuba edingekayo futhi amasampula angashiswa ngqo ekamelweni elivaliwe;
• Ukukhiqiza kabusha okuthuthukisiwe kanye nokuzinza: ngokulawula ngokunembile izinga lokushisa nesikhathi sokushisa, ukuguquguquka kwesampula kuyahambisana kakhulu, kunciphisa amaphutha okusebenza;
• Ukugwema ukungcola noma ukulimala kwekholomu: ingxenye yegesi kuphela efakwa ohlelweni lwe-chromatography, okunciphisa kakhulu ukuphazamiseka kwezingxenye ezingashintshi nekholomu kanye ne-detector.
• Ifanele ukuhlaziywa okuzenzakalelayo: uhlelo lokujova lwe-headspace lungaxhunywa kalula ku-autosampler, olufanele izidingo zokuthola i-throughput ephezulu.

Kodwa-ke, isitsha sesampula esizinzile nesithembekile, ama-headspace vials, sibalulekile ekuhlaziyweni kwe-headspace okusebenzayo nokunembile, okungagcini nje ngokulawula ukuziphatha kokuguquguquka kanye nomphumela wokuvala isampula, kodwa futhi okuthinta ngqo imiphumela yokuhlaziya kokugcina.

Incazelo kanye nemiphumela yama-Headspace Vials

Endleleni yokuqoqa amasampula e-headspace, ukushisa kanye nokuguquguquka kwesampula kanye nenqubo yokuthola isikhala segesi kokubili kwenzeka emabhodleleni e-headspace njengezitsha ezingangenisi moya, nakuba kubonakala kulula, kodwa ukwakheka kanye nokusebenza kwamabhodleleni e-headspace kunomthelela omkhulu ekuthembekeni kwenqubo yonke yokuhlaziya.
Ama-headspace vials ayisampula yamavolumu aklanyelwe ukujova i-headspace ku-gas chromatography. Ukwakhiwa kwawo okuvamile kuqukethe izingxenye ezilandelayo:

Ibhodlela: ngokuvamile yenziwe ngengilazi ye-borosilicate ephezulu, enokumelana okuhle nokushisa okuphezulu kanye nokungangeni kwamakhemikhali, evame ukutholakala ngamavolumu ayi-10ml, 20ml, noma amakhulu;

Ukuvula/intambo yebhodlela: ukuvulwa okujwayelekile okungu-20mm, okufanelekela ama-cap e-aluminium kanye nezinhlelo zokuthatha amasampula ngokuzenzakalela;

Isivalo: ngokuvamile kucindezelwa ngezinto ezihambisanayo ukuqinisekisa ukuqina kwebhodlela;

I-Gasket: kukhona ukwakheka kwezinto ezihlanganisiwe ze-PTFE kanye ne-silicone, ezinokumelana okuhle nokushisa okuphezulu kanye nokungangeni kwamakhemikhali, zingamelana nokubhobozwa okuningi ngaphandle kokuvuza.

Indima eyinhloko yebhodlela le-headspace ukuhlinzeka ngendawo evaliwe, engasebenzi futhi elawulwayo, ukuthi izinyibilikisi eziguquguqukayo kusampula ngaphansi kwezimo zokushisa yindlela oh ibhodlela elingaphezu kwesikhala segesi, ukwakheka kokulingana kwegesi okumelela ukuhlushwa kwe-solvent kusampula yokuqala.

Ngokukhethekile, indima yayo ibonakala kulezi zici ezilandelayo:

Isiqinisekiso sokuvala: ukuvala okuhle ukuqinisekisa ukuthi isampula enkambisweni yokushisa noma yokuphumula ngeke ihlale ibangelwa ukuvuza nokulahleka kwe-solvent;

Ukuvikelwa kwezinto ezingasebenzi: izinto zeglasi kanye ne-gasket ezisezingeni eliphezulu zivimbela ukusabela ngesampula noma i-solvent, zigwema ukwethulwa kwezinto ezingamanga noma ukuphazamiseka kwesignali;

Izimo zevolumu ezihlala njalo: amabhodlela ajwayelekile anegalelo ekuzinzeni kwesikhala sekhanda kanye nokuphindaphinda, okwenza kube lula ukulinganisa kanye nokuqhathaniswa kwemiphumela yokuhlaziya.

Ama-vial e-Headspace antipathy asetshenziswa ku-headspace sampler ezenzakalelayo. Ukuhamba komsebenzi kuvame ukuba kanje:

1. Isixazululo sesampula singezwa ebhodleleni le-headspace bese sivalwa;
2. I-autosampler iphakela i-vial ku-module yokushisa ye-thermostatic;
3. Isampula ishiswa ebhodleleni kuze kufike ekushiseni okubekiwe futhi izingxenye eziguquguqukayo ziyathuthela endaweni yekhanda;
4. Inaliti yomjovo ihlaba i-gasket bese idonsa umthamo wegesi endaweni engaphambili;
5. Igesi ifakwa ku-chromatograph yegesi ukuze ihlukaniswe futhi itholakale i-alamu.

Kule nqubo, ukuzinza kwesakhiwo, ukusebenza kokubhoboza i-gasket, kanye nokuvalwa kwama-headspace vials kuhlobene ngqo nokuvumelana kwesampula kanye nokunemba kwemodeli. Ikakhulukazi, ukusetshenziswa kwama-headspace vials ajwayelekile nathembekile ekusebenzeni okuzenzakalelayo kubalulekile ekuqinisekiseni ukuthi inqubo yokuhlaziya isebenza kahle futhi inciphisa amazinga okuhluleka.

Kungani Ama-Headspace Vials Ebalulekile?

Nakuba i-chromatograph yegesi kanye ne-detector kuyizinto eziyinhloko ekuhlaziyweni kwe-solvent esele, indima ye-headspace vial ibaluleke ngokulinganayo. Njengomthwali we-analytes kusukela ekwelashweni kwesampula ngaphambi kokufakwa, ukusebenza kwayo kuhlobene ngqo nokuzinza kwesistimu yonke yokuhlaziya kanye nokuthembeka kwedatha.

1. Isampula yobuqotho kanye nokulawula ukuguquguquka

Izinyibilikisi ezisele ikakhulukazi ziyizinhlanganisela ezibila kancane, eziphilayo eziguquguqukayo ezisengozini enkulu yokulahlekelwa ngesikhathi sokuchayeka, ukushisa noma ukugcinwa. Uma ama-headspace vials engagcinwanga evalwe ngokuqinile kulo lonke umjikelezo wokuhlaziya, okuqukethwe kwesinyibilikisi kungashintsha, okuholela emiphumeleni echemile.

Ama-headspace vials asezingeni eliphezulu angashiswa abe ngaphezu kuka-100-150°C esimweni esivaliwe, okuqinisekisa ukuthi izingxenye eziguquguqukayo zikhishwa futhi zihlaziywe kuphela ngaphansi kwezimo ezibekiwe;

Ukulawulwa okunembile kwesampula ukuze kufinyelelwe ukulingana kwegesi noketshezi ekushiseni okulinganayo kanye nevolumu kukhulisa ukunemba kanye nokuphindaphindeka kwemiphumela.

2. Ithonya lokusebenza kokuvala emiphumeleni yokuhlaziya

Uhlelo lokuvala ivivali le-Headspace luvame ukuba nezingxenye ezintathu: isivalo, i-gasket kanye ne-mouthpiece. Ukuvala okungekuhle kunoma iyiphi indawo kungabangela ukuvuza kwesampula, umsindo wangemuva ophakeme, noma ngisho nokungcola kwesampula.

Ama-gasket e-PTFE/silicone asezingeni eliphezulu awagcini nje ngokumelana namazinga okushisa aphezulu namakhemikhali, kodwa futhi angamelana nokubhoboza okuningi futhi agcine ukuvalwa okuhle;

I-gasket esezingeni eliphansi noma i-gland ekhululekile ingabangela ukuthi i-solvent iphume ngaphambi kokuhlaziywa noma ngesikhathi sokushisa, okuthinta ngqo indawo ephakeme futhi kunciphisa ukunemba kwenani.

3. Ukuhambisana nezinhlelo zokuhlola ngokuzenzakalela

Ama-injector e-headspace azenzakalelayo avame ukusetshenziswa emalabhorethri esimanje ukuthuthukisa ukusebenza kahle kanye nokuvumelana kwemiphumela, futhi ukwakheka okujwayelekile kwe-Headspace vial kuvumela ukuthi ivumelane ngqo nemikhiqizo emikhulu yezinhlelo zokujova.

Ubukhulu obujwayelekile buqinisekisa ukuthi amabhodlela angabonakala ngokuzenzakalelayo, abekwe kahle futhi abhobozwe ku-injector;

Ukunciphisa amaphutha enziwe ngesandla kuthuthukisa ukusebenza kahle kokucubungula amasampula kanye nokuvumelana kwedatha, okwenza i-Headspace vial ifaneleke kakhulu ezimweni zokuhlola ezisebenzisa i-high-throughput.

4. Ukungangeni kahle kwezinto zamakhemikhali

Amakhemikhali amabhodlela nezinto zokuvala akufanele ashaywe indiva lapho kuhlaziywa izincibilikisi ezilandelanayo. Izinto ezisezingeni eliphansi zingase zimunce noma zisabele ngama-molecule ezincibilikisi, okuholela emiphumeleni echemile.

Ingilazi ye-borosilicate ayisebenzi ngamakhemikhali futhi izinzile ngokwezinga lokushisa, ivimbela ukumuncwa kwe-solvent noma ukuwohloka kwezinga lokushisa;

Kwezinye izinhlelo ezikhethekile zokuncibilikisa, ama-gasket enziwe ngezinto ezikhethekile ayadingeka ukuqinisekisa ukuzwela kokutholwa kanye nokuqina kwesampula.

I-Headspace vial ayiyona nje isitsha esilula sesampula, iyisici esibalulekile ekuqinisekiseni ukuthi imiphumela yokuhlaziywa kwe-solvent esele iyiqiniso, iyahambisana futhi iyaphindaphindeka. Ithatha imisebenzi eminingi ebalulekile kulo lonke uchungechunge lokuhlaziya, njengokuvikela ukuvala, ukulawula ukuguquguquka, ukufanisa uhlelo, isiqinisekiso sokungasebenzi kahle kwamakhemikhali, njll. Ingenye yezinto ezingasetshenziswa esikhundleni sazo ukuze kufezwe ukuhlolwa kwezidakamizwa okuseqophelweni eliphezulu.

Izici Ezibalulekile Ekukhetheni I-Headspace Vial Efanele

Ekuhlaziyweni kwe-solvent eseleyo, ukukhethwa kwe-headspace vial efanele kuyimfuneko ukuqinisekisa ukunemba kwedatha kanye nokuvumelana kwendlela. Izidingo ezahlukene zokuhlola, izinhlobo zamasampula kanye namapulatifomu ezinsimbi anezidingo ezahlukene zezinto ze-headspace vial, isakhiwo kanye nokusebenza. Izici ezilandelayo ezibalulekile kufanele zicatshangelwe lapho ukhetha i-headspace vial:

1. Izinto: uhlobo lwengilazi kanye nokucaca

• Ingilazi ye-borosilicate yekilasi lokuqala: into ethandwa kakhulu yebhodlela yokuhlaziya i-solvent esele. Ukumelana kwayo okuhle kakhulu nokushisa namakhemikhali kanye nokuhlushwa kwayo okuphansi kakhulu kwama-ion aqhumile kuvimbela ukusabela kwamakhemikhali phakathi kwe-solvent nebhodlela, kugwema imiphumela engamanga noma ukuphazamiseka kwesignali.
• Ukucaca okuphezulu kwebhodlela: ivumela ukubonwa okusheshayo kwesimo sesampula ngesikhathi sokuskena, ukuhlola noma ukuhlola ikhwalithi, njengokuba khona kwama-precipitate, inani eliqondile loketshezi, njll., kanye nokuhlonza kalula izinhlelo ezenzakalelayo.

2. Ukukhetha ivolumu: imininingwane evame ukusetshenziswa 10ml, 20ml

Ukukhethwa komthamo we-Headspace vial kufanele kusekelwe enhlanganisela yalezi zici ezilandelayo:

• Ivolumu yesampula: Ngokuvamile ivolumu yesampula icishe ibe ngu-50% wevolumu yebhodlela ukuqinisekisa isikhala esanele sekhanda (indawo yegesi) sokulingana kokuguquguquka;
• Izidingo Zendlela YokuhlaziyaIsibonelo, indlela ye-USP <467> ye-solvent eseleyo incoma ukusetshenziswa kwebhodlela le-headspace elingu-20 ml;
• Ukuhambisana kwe-Autosampler: qinisekisa ukuthi ibhodlela elikhethiwe lisekela imodeli yethuluzi elisetshenzisiwe, ikakhulukazi ibhodlela elingaphezu komgodi.

3. Uhlobo lwe-gasket yesembozo: ukuvala kanye nokufaneleka kwamakhemikhali

Izinto ze-gasket: esetshenziswa kakhulu yi-PTFE composite gasket, isakhiwo sayo esinezingqimba ezimbili sihlanganisa i-inertia yamakhemikhali ye-PTFE nokuqina kokuvalwa kwe-silicone, singamelana nokubhoboza kwezinga lokushisa eliphezulu futhi sigcine ukuvalwa okuhle; ukuze uthole izinyibilikisi ezinamandla ezibolayo noma ezinkulu, ungakhetha i-PTFE layer reinforced gasket ehlanzekile kakhulu.

Izinhlobo zezivalo zamabhodlela: Ama-cap e-aluminium afanelekela iningi lamathuluzi, ane-gland eqinile kanye nokuvala okuhle kakhulu; Ama-cap e-magnetic afanelekela izinhlelo zokuthatha amasampula ngokuzenzakalela ezinokuhlonza i-magnetic, okusiza ukuthuthukisa ukusebenza kahle kokudla kanye nokunemba kokubeka; Ama-cap anezintambo, yize elungele ukusebenza ngesandla, angase angavali kahle izinhlobo zama-gland futhi afaneleka kakhulu ezigabeni zokukhula noma izimo ezingezona eziphezulu.

4. Ukucatshangelwa kokusetshenziswa kabusha kanye nezindleko

Ama-vial engilazi angasetshenziswa kabusha (adinga ukuhlanzwa nokuhlanza okushisa okuphezulu) afanelekela ezinye izindlela ezingezona ezemithi noma izifundo zokuthuthukisa futhi anganciphisa izindleko zesikhathi eside;

Kodwa-ke, ekukhiqizweni kwe-GMP noma emalabhorethri okulawula ikhwalithi asemthethweni, amabhodlela asetshenziswa kanye angcono ekuqinisekiseni ukuhlanzeka nokugwema ukungcoliswa okuhlukahlukene;

Uma uthenga ngamaqoqo, kubalulekile futhi ukukala ikhwalithi yomkhiqizo, ukuhambisana kweqoqo ngalinye, kanye nentengo ukuze ukhethe umhlinzeki onikeza ibhalansi yokusebenza kanye nezindleko.

Ukukhetha okunengqondo kwe-headspace vial akuyona nje into eyisisekelo, kodwa futhi kuyindlela yokubonisa ukuqonda ukulawula ikhwalithi. Ukukhetha ngakunye kwamapharamitha okubonakala kuncane kudlala indima ebalulekile ekunembeni kwemiphumela, ukuzinza kwesistimu kanye nokusebenza kahle kwelabhorethri. Ngakho-ke, ukuqonda okujulile kwalezi zici ezibalulekile kuyikhono elibalulekile lochwepheshe kubo bonke ochwepheshe abasebenza ekuhlaziyeni kwemithi.

Imibuzo Evame Ukubuzwa Namanothi

Nakuba ama-headspace vials esetshenziswa kabanzi ekuhlaziyeni i-residue solvent, uchungechunge lwezinkinga lungavela ngokoqobo ngenxa yokuphathwa kabi noma ukukhetha izinto ezisetshenziswayo. Nazi izinkinga ezivamile kanye nezincomo zokuvimbela:

1. Indlela yokugwema ukungcoliswa kwesampula

Ukungcola okuxubile akugcini nje ngokuthinta ukunemba kwemiphumela yokuhlaziya, kodwa futhi kungabangela ukuphazamiseka okufihliwe kwesikhathi eside ohlelweni lokuthola, ikakhulukazi engozini enkulu lapho kuhlaziywa amazinga aphansi. Izinyathelo ezilandelayo zingayigwema ngempumelelo le nkinga:

• Beka phambili ukusetshenziswa kwama-vial alahlwayo nama-cap pad: lena yindlela eqondile nephumelelayo kakhulu, ikakhulukazi ekulawulweni kwekhwalithi yemithi kanye nokuhlolwa komthetho;
• Shintsha noma uhlanze kahle ama-vial asetshenziswe kabusha: uma kudingeka ukusetshenziswa kabusha, qiniseka ukuthi zihlanzwe kahle kusetshenziswa izinyathelo ezifana namanzi ahlanziwe, izinyibilikisi eziphilayo, kanye nokomisa okushisa okuphezulu;
• Imikhuba yokusabalalisa ngokuqinile: sebenzisa amathuluzi akhethekile okufaka amapayipi ukuze ugweme ukuconsa kwesampula ebhodleleni noma eduze kwalo;
• Hlanza izivalo zamabhentshi namabhantshi amathuluzi: uma uphatha izinyibilikisi ezishintshashintshayo, amagilavu ​​​​kufanele ashintshwe njalo ukuze kuvinjelwe ukusabalala kokungcola ngokuphatha.

2. Ukuvuza kwesivalo ngesikhathi sokushisa

Ekuhlaziyweni kwesikhala sekhanda, isampula idinga ukushiswa ku-80-120°C noma ngaphezulu. Uma izivalo noma ama-gaskets engavaliwe kahle, izinyibilikisi zingaphuma ngesikhathi senqubo yokushisa, okuholela ekushintshashintsheni kwedatha noma imiphumela ephansi.

• Khetha ama-gasket asezingeni eliphezulu: kufanele zibe nokumelana okuhle nokushisa kanye nokuqina kokubhoboza ukuqinisekisa ukuthi isivalo asikhululeki;
• Amandla okuvala afanele: isivalo esenziwe ngesandla noma esenziwa ngokuzenzakalelayo sidinga ukuba silinganiselwe, ukukhululeka kakhulu kungavuza, kuqine kakhulu kungalimaza i-gasket noma kubangele ukuthi ibhodlela liqhume;
• Ukuhlolwa njalo kwenaliti yesistimu yokudla: inaliti egugile noma ekhubazekile ingavimbela i-gasket ukuthi ingazivali, okuholela ekuvuzeni;
• Ukusetha izinga lokushisa okunengqondo: akufanele kudlule umkhawulo ophezulu wokumelana nokushisa kwe-gasket noma i-cap, ngokuvamile kulawulwa ebangeni elingu-110-130 ℃ kuphephile.

3. Izincomo zokuhlanza nokugcina amabhodlela

Ukuze kusetshenziswe kabusha amabhodlela okungenzeka ukuthi kuhileleke esigabeni sokulawula izindleko noma sokuthuthukiswa kwendlela, kudingeka kuqashelwe kakhulu imikhuba yokuhlanza nokugcina ukuze kugwenywe ukufakwa kokungcola noma izincibilikisi ezisele:

• Izinyathelo zokuhlanza eziphakanyisiwe: hlanza izikhathi eziningana ngamanzi ahlanzekile; hlanza ngezithako zemvelo ezifanele; ukuhlanza nge-ultrasound kuye ngokuthi ukungcola kungakanani; ukomisa ngezinga lokushisa eliphezulu ku-105℃-120℃ ukuqinisekisa ukuthi akukho umswakama noma isithako esisele.
• Izincomo zesitoreji: indawo yokugcina ehlanzekile, eyomile nevaliwe, ukugwema uthuli, izinto ezishintshashintshayo zingaphinde zingcolise; ngaphambi kokusebenzisa uma zigcinwe isikhathi eside kakhulu, kunconywa ukuthi uphinde uhlole futhi uhlanze futhi; gwema ukuchayeka isikhathi eside elangeni noma ekushiseni okuphezulu, ukuvimbela ukuguga kwengilazi noma i-gasket.

Ngokwazi kahle le mininingwane ebalulekile yokusebenza, awukwazi nje ukuthuthukisa ukunemba nokuphindeka kokuhlolwa, kodwa futhi wandise ngempumelelo impilo yesevisi yemishini futhi unciphise izinga lokwehluleka. Ezintweni zokuhlaziya ezifana nezincibilikisi ezisele, ezizwela kakhulu ekushintsheni kokulandelela, ukuphathwa okuningiliziwe kwesixhumanisi ngasinye sokusebenza akufanele kunganakwa.

Isiphetho

Ensimini elawulwa kakhulu futhi enembile yokuhlaziywa kwe-solvent yezinsalela zemithi, i-headspace vial, nakuba incane, idlala indima ebalulekile nebalulekile. Kusukela ekugcinweni, ekuvaleni nasekufudumaleni kwesampula, kuya ekuxhumaniseni nohlelo lwe-autosampling, kuyindlela yokuqala yokuzivikela kulo lonke uchungechunge lokuhlaziya ukuqinisekisa ukusebenza kwedatha.

Ama-headspace vials asezingeni eliphezulu awagcini nje ngokuvikela ubuqotho besampula, avimbele ukulahlekelwa ukuguquguquka, futhi athuthukise ukuhambisana komjovo, kodwa futhi ayisisekelo esidingekayo sokutholwa okuphindaphindwayo nokubucayi kakhulu ekuhlaziyweni okuzenzakalelayo. Ikakhulukazi lapho kubhekene nokuhlaziywa kwenani lezinga lokulandelela okudingekayo yizindinganiso ze-pharmacopoeia, iphutha elincane le-cap, izinto ezingafanele, noma ngisho nokusebenza kokugcwalisa isampula okungenangqondo kuzoba nomthelela ongelutho emiphumeleni yokuhlaziya.

Njengoba ukuthuthukiswa kwezidakamizwa kanye nokulawulwa kwekhwalithi kuqhubeka nokwandisa izinga lokuzenzakalela kanye nokutholwa, amazinga ekhwalithi ama-headspace vials nawo ayaphakanyiswa. Kusukela ekuhlanzekeni kwezinto ezibonakalayo, ukuhambisana kwegama kuya ekuvumelaneni kwesistimu, ama-headspace vials esikhathi esizayo akufanele nje abe azinzile futhi athembeke, kodwa futhi adlale indima "ye-interface ejwayelekile" elabhorethri yokuhlela, esiza ekulandeleni idatha, ukukhiqizwa kabusha kwendlela kanye nokuthuthukiswa okuqhubekayo kokulawulwa kwekhwalithi.