Intshayelelo

Kwinkqubo yokuvelisa amayeza, izinyibilikisi zisetyenziswa kakhulu kwiinkalo ezininzi zokwenziwa kwe-API, ukukhupha, ukucoca kunye neenkqubo zokwenziwa. Nangona kunjalo, ukuba ezi zinyibilikisi zendalo azisuswanga ngokupheleleyo kwimveliso yokugqibela, kuya kwenziwa “izinyibilikisi eziseleyo”. Ezinye izinyibilikisi zinetyhefu, umhlaza okanye ezinye iingozi zempilo ezinokubakho, ngoko ke, ulawulo oluqinileyo lomxholo wezinyibilikisi eziseleyo kwimithi ayisiyiyo nje ikhonkco eliphambili lokuqinisekisa ukhuseleko lwamayeza ezigulana, kodwa ikwayinxalenye ebalulekileyo yolawulo lomgangatho wamayeza.

Kuhlalutyo lwe-headspace, isampuli ivalwa kwisitya esithile ukuze ifudumale, ukuze izinto eziguquguqukayo zikhutshwe kwindawo yegesi engaphezulu kwesikhongozeli, ize emva koko le gesi ifakwe kwi-chromatograph yegesi ukuze ihlalutywe. Ukuthembeka nokuchaneka kweli nyathelo libonakala lilula kuxhomekeke kakhulu kwizixhobo ezibalulekileyo ezisetyenziswayo – ii-headspace vials.

Isishwankathelo seendlela zohlalutyo lwe-Residual Solvent

Iindidi ngeendidi zezinyibilikisi ezisele ezikhoyo kumayeza, ezineempawu ezahlukeneyo zetyhefu, kufuneka zihlelwe ngokwamaqela kwaye zilawulwe ngokweengozi zazo ezinokubakho xa zihlalutywa kwaye zilawulwa. Izikhumbuzo zokuhlelwa eziphononongwa ngontanga zamazwe ngamazwe zihlela izinyibilikisi ezisele kwiindidi ezintathu ezilandelayo:

1. Udidi 1: Izinyibilikisi ezingavumelekanga

Kuquka i-benzene, i-methylene chloride, i-1,2-dichloroethane, i-carbon tetrachloride, njl.njl., ezinokubangela umhlaza omkhulu kunye neengozi kwindalo, kufuneka ziphetshwe kwinkqubo yemveliso. Imida ilawulwa kakhulu kwaye idla ngokubalwa kumanqanaba e-ppm okanye angaphantsi.

2. Udidi 2: Izinyibilikisi zilawulwa ngokulinganiselweyo

Kubandakanya i-toluene, i-acetonitrile, i-DMF, i-isopropyl alcohol njalo njalo. Ubudala bezi zinyibilikisi buyamkeleka phantsi kwemida ethile, kodwa zisenemingcipheko ethile yetyhefu. Imida ibekwa ngokusekelwe kwi-ADI kwaye idla ngokufuna ukubekwa esweni ngokungqongqo.

3. Udidi 3: Izinyibilikisi ezinetyhefu ephantsi

Ezi ziquka i-ethanol, i-propanol, i-ethyl acetate, njl.njl., ezinobungozi obuphantsi ebantwini kwaye ngokubanzi zithathwa njengezikhuselekileyo kumayeza ukuya kuthi ga kwi-50 mg yemihla ngemihla.

Ukuze kuchongwe ngokuchanekileyo uhlobo kunye nomxholo wezi solvents ezisele, i-gas chromatography (GC) okwangoku yeyona ndlela iphambili yohlalutyo, enezibonelelo ezibalulekileyo zobuntununtunu obuphezulu, ukusebenza kakuhle kokwahlulwahlulwa, kunye nokusetyenziswa kwiikhompawundi eziguquguqukayo, ezinokuhlangabezana neemfuno zohlalutyo lwe-solvent ezisele ukuze kufunyanwe umkhondo.

Phakathi kweendlela ezahlukeneyo zokujova ze-chromatography yemozulu, iteknoloji yokujova ye-headspace isetyenziswa kakhulu ekufumaneni izinyibilikisi ezisele kwimithi. Iteknoloji ngokusebenzisa uthando lwesampuli evalwe kwibhotile ye-headspace, eshushu ukuya kubushushu obufanelekileyo, sisinyibilikisi esikwi-volatilization yesampuli singene kwindawo yegesi yebhotile, size emva koko siphume kwindawo ukuze kukhutshwe umthamo othile wegesi eqeshisiweyo kwi-GC ukuze ihlalutywe.

Iingenelo zokutyala intloko ziquka:

• Unyango lwangaphambi konyango oluncitshisiweyo: akukho msebenzi wokukhupha isinyibilikisi okanye wokuxuba onzima ofunekayo kwaye iisampulu zinokufudunyezwa ngqo kwigumbi elivaliweyo;
• Ukuphucula ukuzala kwakhona kunye nozinzo: ngokulawula ngokuchanekileyo ubushushu bokufudumeza kunye nexesha, ukuguquguquka kwesampulu kuyafana ngakumbi, kunciphisa iimpazamo zokusebenza;
• Ukuphepha ungcoliseko okanye umonakalo kwikholamu: yinxenye yegesi kuphela efakwa kwinkqubo ye-chromatography, nto leyo enciphisa kakhulu ukuphazamiseka kwezinto ezingezizo ezonakalayo kwikholamu kunye nesixhobo sokufumanisa.
• Ifanelekile kuhlalutyo oluzenzekelayo: inkqubo yokufaka i-headspace inokuthi iqhagamshelwe ngaphandle komthungo kwi-autosampler, ifanele iimfuno zokufumanisa i-flowput ephezulu.

Nangona kunjalo, isikhongozeli sesampulu esizinzileyo nesithembekileyo, ii-headspace vials, sibalulekile kuhlalutyo olusebenzayo noluchanekileyo lwe-headspace, olungalawuli kuphela indlela yokuziphatha kwe-volatilization kunye nefuthe lokutywina kwesampulu, kodwa lukwachaphazela ngokuthe ngqo iziphumo zohlalutyo lokugqibela.

Inkcazo kunye neziphumo zeeVials zeHeadspace

Kwindlela yokuvavanya i-headspace, ukufudumeza kunye nokuguquguquka kwesampuli kunye nenkqubo yokufumana isithuba segesi zombini zenzeka kwii-headspace vials ezifana nezikhongozeli ezingangeni moya, nangona kubonakala kulula, kodwa uyilo kunye nokusebenza kwee-headspace vials kunempembelelo enkulu ekuthembekeni kwenkqubo yonke yohlalutyo.
Iibhotile ze-Headspace ziyimiqulu yesampulu eyenzelwe ukufakwa kwe-headspace kwi-gas chromatography. Ulwakhiwo lwayo oluqhelekileyo luquka ezi nxalenye zilandelayo:

Ibhotile: ngokubanzi yenziwe ngeglasi ye-borosilicate ephezulu, enokumelana okuhle nobushushu obuphezulu kunye nokungasebenzi kakuhle kweekhemikhali, efumaneka rhoqo kwi-10ml, 20ml, okanye imiqulu emikhulu;

Ukuvula ibhotile/umsonto: ubukhulu becala ukuvulwa okuqhelekileyo kwe-20mm, okufanelekileyo kwiikhaphu ze-aluminium kunye neenkqubo ze-autosampling;

Ikepusi: idla ngokucinezelwa ngezinto ezihambelanayo ukuqinisekisa ukuqina kwebhotile;

I-Gasket: kukho ukwakheka kwezinto ezidityanisiweyo ze-PTFE kunye ne-silicone, ezinokumelana okuhle nobushushu obuphezulu kunye nokungasebenzi kakuhle kweekhemikhali, zinokumelana nokugqobhozwa okuninzi ngaphandle kokuvuza.

Indima ephambili yebhotile ye-headspace kukubonelela ngendawo evaliweyo, engasebenziyo nelawulwayo, kukuba izinyibilikisi eziguquguqukayo kwisampuli phantsi kweemeko zokufudumeza yindlela oh ibhotile engaphezulu kwendawo yegesi, ukwakheka komlinganiselo wegesi omele uxinzelelo lwe-solvent kwisampuli yokuqala.

Ngokukodwa, indima yayo ibonakala kwezi zinto zilandelayo:

Isiqinisekiso sokutywina: ukutywinwa kakuhle ukuqinisekisa ukuba isampuli kwinkqubo yokufudumeza okanye yokuphumla ayizukubangwa kukuvuza kunye nokulahleka kwesinyibilikisi;

Ukhuseleko lwezinto ezingasebenziyo: izixhobo zeglasi kunye ne-gasket ezikumgangatho ophezulu zithintela ukusabela kwisampuli okanye kwisinyibilikisi, ziphepha ukungeniswa kwezinto ezingezizo okanye ukuphazamiseka kwesignali;

Iimeko zevolumu ezihlala zihleli: iibhotile ezisemgangathweni zinegalelo ekuzinzeni kwendawo yentloko kunye nokuphindaphinda, okwenza kube lula ukulinganisa kunye nokuthelekiswa kweziphumo zohlalutyo.

Iibhotile ze-Headspace ezichasene nokuphelelwa lithemba ezisetyenziswa kwisampulu ye-headspace ezenzekelayo. Umsebenzi uhlala ngolu hlobo lulandelayo:

1. Isisombululo sesampulu songezwa kwi-headspace vial size sivalwe;
2. I-autosampler yondla ibhotile kwimodyuli yokufudumeza ye-thermostatic;
3. Isampuli itshiswa kwi-vial ukuya kubushushu obumiselweyo kwaye izinto eziguquguqukayo ziyafudukela kwindawo yentloko;
4. Inaliti yokujova ihlaba i-gasket ize ikhuphe umthamo wegesi kwindawo eyintloko;
5. Igesi ifakwa kwi-chromatograph yegesi ukuze yahlulwe kwaye ifunyanwe yi-alamu.

Kule nkqubo, uzinzo lwesakhiwo, ukusebenza kokubhoboza i-gasket, kunye nokutywinwa kwee-headspace vials kunxulumene ngokuthe ngqo nokuhambelana kwesampulu kunye nokuchaneka komzekelo. Ngokukodwa, ukusetyenziswa kwee-headspace vials ezisemgangathweni nezithembekileyo kwimisebenzi ezenzekelayo kubalulekile ekuqinisekiseni ukuba inkqubo yohlalutyo isebenza kakuhle kwaye inciphisa amazinga okusilela.

Kutheni iiVili zeHeadspace zibalulekile?

Nangona i-gas chromatograph kunye ne-detector zezona zixhobo ziphambili kuhlalutyo lwe-residual solvent, indima ye-headspace vial ibaluleke ngokulinganayo. Njengomthwali we-analytes ukusuka kwisampuli yonyango lwangaphambi kokusetyenziswa ukuya kwi-injection, ukusebenza kwayo kunxulumene ngokuthe ngqo nokuzinza kwenkqubo yonke yohlalutyo kunye nokuthembeka kwedatha.

1. Isampulu yokuthembeka kunye nolawulo lokuguquguquka

Izinyibilikisi eziseleyo ikakhulu ziikhompawundi ezibila kancinci, eziguquguqukayo zendalo ezisengozini enkulu yokulahleka ngexesha lokuvezwa, ukufudumeza okanye ukugcinwa. Ukuba ii-headspace vials azigcinwanga zivaliwe ngokuqinileyo kulo lonke umjikelo wohlalutyo, umxholo wesinyibilikisi unokutshintsha, nto leyo ekhokelela kwiziphumo ezingathathi cala.

Iibhotile zentloko ezikumgangatho ophezulu zinokufudunyezwa zibe ngaphezu kwe-100-150°C xa zivaliwe, ukuqinisekisa ukuba izinto eziguquguqukayo zikhutshwa kwaye zihlalutywe kuphela phantsi kweemeko ezimiselweyo;

Ulawulo oluchanekileyo lwesampuli ukuze ifikelele kumlinganiselo wegesi-ulwelo kubushushu obungaguqukiyo kunye nomthamo kwandisa ukuchaneka kunye nokuphindaphinda kweziphumo.

2. Impembelelo yokusebenza kokutywina kwiziphumo zohlalutyo

Inkqubo yokutywina i-Headspace vial idla ngokuba namacandelo amathathu: isiciko, i-gasket kunye ne-mouthpiece. Ukutywina okungekho semgangathweni nangaliphi na ixesha kunokubangela ukuvuza kwesampuli, ingxolo ephezulu yangasemva, okanye nokuba isampuli ingcoliswe.

Iigasket zePTFE/silicone ezikumgangatho ophezulu azimelani nje kuphela nobushushu obuphezulu kunye neekhemikhali, kodwa zinokumelana nokubhoboka okuninzi kwaye zigcine isitywino esihle;

I-gasket esemgangathweni ophantsi okanye i-gland ekhululekileyo inokubangela ukuba i-solvent iphume ngaphambi kohlalutyo okanye ngexesha lokufudumeza, nto leyo echaphazela ngqo indawo encotsheni kwaye inciphise ukuchaneka kobungakanani.

3. Ukuhambelana neenkqubo zokwenza iisampulu ngokuzenzekelayo

Ii-injectors ze-headspace ezizenzekelayo zisetyenziswa kakhulu kwiilebhu zanamhlanje ukuphucula ukusebenza kakuhle kunye nokuhambelana kweziphumo, kwaye uyilo oluqhelekileyo lwe-Headspace vial luvumela ukuba ilungelelaniswe ngokuthe ngqo kwiimpawu eziphambili zeenkqubo zokujova.

Ubukhulu obumiselweyo buqinisekisa ukuba iibhotile zinokuchongwa ngokuzenzekelayo, zibekwe ngokuchanekileyo kwaye zibhobozwe kwi-injector;

Ukunciphisa iimpazamo ezenziwe ngesandla kuphucula ukusebenza kakuhle kokucubungula iisampulu kunye nokuhambelana kwedatha, okwenza i-Headspace vial ifaneleke kwiimeko zovavanyo oluphezulu.

4. Ukungangeni kakuhle kweekhemikhali kwezinto

Ikhemikhali yeebhotile kunye nezinto zokutywina akufuneki ijongwe xa kuhlalutywa izinyibilikisi ezincinci. Izinto ezisemgangathweni ophantsi zinokufunxa okanye zenze iimolekyuli zesinyibilikisi, nto leyo ekhokelela kwiziphumo ezithambekele ecaleni.

Iglasi ye-borosilicate ayisebenzi ngokweekhemikhali kwaye izinzile ngokwee-thermal, ithintela ukufunxwa kwe-solvent okanye ukuwohloka kobushushu;

Kwiinkqubo ezithile zesinyibilikisi ezikhethekileyo, ii-gasket ezenziwe ngezinto ezikhethekileyo ziyafuneka ukuqinisekisa ukuba ziyafumaneka kwaye zizinzile kwisampuli.

I-Headspace vial ayisiyonto nje elula yesampulu, iyinxalenye ebalulekileyo ekuqinisekiseni ukuba iziphumo zohlalutyo lwe-solvent eseleyo ziyinyani, ziyafana kwaye ziyaphindaphindeka. Ithatha imisebenzi emininzi ebalulekileyo kulo lonke uthotho lohlalutyo, njengokukhusela ukutywina, ulawulo lwe-volatilization, ukuhambelana kwenkqubo, isiqinisekiso sokungangeni kweekhemikhali, njl. Yenye yezinto ezingasetyenziswa endaweni yazo ukuze kufezekiswe uvavanyo lwamayeza olusemgangathweni ophezulu.

Izinto ezibalulekileyo ekukhetheni iVial yeHeadspace efanelekileyo

Kuhlalutyo lwe-residue solvent, ukukhethwa kwe-headspace vial efanelekileyo kuyimfuneko ukuqinisekisa ukuchaneka kwedatha kunye nokuhambelana kwendlela. Iimfuno ezahlukeneyo zovavanyo, iintlobo zeesampuli kunye namaqonga ezixhobo aneemfuno ezahlukeneyo zezinto ze-headspace vial, ulwakhiwo kunye nokusebenza. Ezi zinto zilandelayo ziphambili kufuneka ziqwalaselwe xa ukhetha i-headspace vial:

1. Izinto: uhlobo lweglasi kunye nokubonakala

• Iglasi ye-borosilicate yeklasi yoku-1: izinto zebhotile ezikhethwayo zohlalutyo lwe-solvent eseleyo. Ukumelana kwayo nobushushu kunye neekhemikhali okugqwesileyo kunye noxinzelelo oluphantsi kakhulu lwee-ions ezikhawulezileyo zithintela ukusabela kweekhemikhali phakathi kwe-solvent kunye nebhotile, ziphepha ubuxoki okanye ukuphazamiseka kwesignali.
• Ukukhanya okuphezulu kwebhotile: ivumela ukujongwa ngokukhawuleza kwesimo sesampulu ngexesha lokutshiza, ukuhlolwa okanye ukujonga umgangatho, njengokubakho kweeprecipitates, ubungakanani obuchanekileyo bolwelo, njl.njl., kunye nokuchongwa lula ziinkqubo ezizenzekelayo.

2. Ukukhetha ivolumu: iinkcukacha ezisetyenziswa rhoqo 10ml, 20ml

Ukukhethwa komthamo we-Headspace vial kufuneka kusekelwe kwindibaniselwano yezi zinto zilandelayo:

• Umthamo wesampulu: Ngokwesiqhelo umthamo wesampulu umalunga ne-50% yomthamo webhotile ukuqinisekisa indawo eyaneleyo yentloko (indawo yegesi) yokulingana kokuguquguquka;
• Iimfuneko zeNdlela yoHlalutyoUmzekelo, indlela ye-USP <467> ye-residual solvent icebisa ukusetyenziswa kwe-20 ml headspace vial;
• Ukuhambelana kwe-Autosampler: qinisekisa ukuba ibhotile ekhethiweyo iyayixhasa imodeli yesixhobo esisetyenzisiweyo, ingakumbi ibhotile engaphezulu kwembobo.

3. Uhlobo lwegasket yesigqubuthelo: ukutywinwa kunye nokufaneleka kweekhemikhali

Izinto ze-gasket: Eyona gasket isetyenziswa kakhulu yi-PTFE composite, isakhiwo sayo esinamaleko amabini sidibanisa i-inertia yeekhemikhali ye-PTFE kunye nokuqina kwe-silicone sealing, inokumelana nokubhobozwa kobushushu obuphezulu kwaye igcine ukutywinwa okuhle; kwizinyibilikisi ezinamandla okanye ezinkulu, ungakhetha i-gasket eqinisiweyo ye-PTFE ecocekileyo kakhulu.

Iintlobo zezivalo zebhotile: Izivalo ze-aluminium zifanelekile kwizixhobo ezininzi, ezine-gland eqinileyo kunye nokuvala okugqwesileyo; Izivalo ze-magnetic zifanelekile kwiinkqubo ze-autosampling ezine-magnetic identification, enceda ukuphucula ukusebenza kakuhle kokutya kunye nokuchaneka kokubeka; Izivalo ezinemisonto, nangona zilungele ukusetyenziswa ngesandla, zisenokungavali kakuhle kwiintlobo ze-gland kwaye zifanelekile ngakumbi kwizigaba zophuhliso okanye kwiimeko ezingezizo eziphezulu.

4. Ukuqwalaselwa kokusetyenziswa kwakhona kunye neendleko

Iibhotile zeglasi eziphinda zisetyenziswe (ezifuna ukucocwa nokubulawa iintsholongwane ngobushushu obuphezulu) zifanelekile kwezinye iindlela ezingezizo ezemithi okanye izifundo zophuhliso kwaye zinokunciphisa iindleko zexesha elide;

Nangona kunjalo, kwimveliso ye-GMP okanye kwiilabhoratri zolawulo lomgangatho ezisesikweni, iibhotile ezisetyenziswa kanye zingcono ukuqinisekisa ucoceko kunye nokuphepha ukungcola okuxutyiweyo;

Xa uthenga ngeebhetshi, kubalulekile nokuvavanya umgangatho wophawu, ukuhambelana kwebhetshi nganye, kunye nexabiso ukuze ukhethe umthengisi obonelela ngokulinganisela ukusebenza kunye neendleko.

Ukukhetha ngengqiqo i-headspace vial akusiyonto ilula nje kuphela, kodwa ikwayindlela yokubonakalisa ukuqonda komgangatho. Zonke iiparameter ezibonakala zincinci zidlala indima ebalulekileyo ekuchanekeni kweziphumo, uzinzo lwenkqubo kunye nokusebenza kakuhle kwelebhu. Ke ngoko, ukuqonda okunzulu kwezi zinto zibalulekileyo sisakhono sobungcali esibalulekileyo kuyo yonke ingcali esebenza kuhlalutyo lwamayeza.

Imibuzo Ebuzwa Rhoqo kunye namanqaku

Nangona ii-headspace vials zisetyenziswa kakhulu kuhlalutyo lwe-residue solvent, uthotho lweengxaki lusenokuvela ngenxa yokuphathwa kakubi okanye ukukhetha izinto ezisetyenziswayo. Ezi zilandelayo ziingxaki eziqhelekileyo kunye neengcebiso zokuthintela:

1. Indlela yokuphepha ukungcoliswa kweesampuli

Ungcoliseko olunqamlezileyo aluchaphazeli kuphela ukuchaneka kweziphumo zohlalutyo, kodwa lunokubangela ukuphazamiseka okufihlakeleyo kwexesha elide kwinkqubo yokufumanisa, ingakumbi kumngcipheko ophezulu xa kuhlalutywa amanqanaba aphantsi. La manyathelo alandelayo anokuyiphepha ngempumelelo le ngxaki:

• Kubaluleke kakhulu ukusetyenziswa kweebhotile kunye neephedi zeesigqubuthelo ezilahlwayo: le yeyona ndlela ithe ngqo nesebenzayo, ingakumbi kulawulo lomgangatho wamayeza kunye novavanyo lolawulo;
• Tshintsha okanye ucoce ngokupheleleyo iibhotile ezisetyenzisiweyo: ukuba kufuneka zisetyenziswe kwakhona, qiniseka ukuba zicociwe kakuhle kusetyenziswa amanyathelo anje ngamanzi acocekileyo, izinyibilikisi zendalo, kunye nokomisa ngobushushu obuphezulu;
• Iindlela ezingqongqo zokusasaza: sebenzisa izixhobo ezikhethekileyo zokufaka imibhobho ukuze ungafumani isampuli ebhotileni okanye ejikeleze yona;
• Coca ii-bench tops kunye neeglavu zezixhobo: xa uphatha izinyibilikisi eziguquguqukayo, iiglavu mazitshintshwe rhoqo ukuthintela ukusasazwa kongcoliseko ngokuphatha.

2. Ukuvuza kwesiciko ngexesha lokufudumeza

Kuhlalutyo lwe-headspace, isampuli kufuneka ifudunyezwe ukuya kuma-80-120°C nangaphezulu. Ukuba ii-caps okanye ii-gaskets azivalwanga kakuhle, izinyibilikisi zinokuphuma ngexesha lenkqubo yokufudumeza, nto leyo ekhokelela ekutshintsheni kwedatha okanye kwiziphumo eziphantsi.

• Khetha ii-gaskets ezikumgangatho ophezulu: kufuneka zibe nokumelana nobushushu okuhle kunye nokugqabhuka okuthambileyo ukuqinisekisa ukuba isitywino asikhululeki;
• Amandla okuvala achanekileyo: isivalo esenziwe ngesandla okanye esizenzekelayo kufuneka sibe phakathi, ukukhululeka kakhulu kunokuvuza, ukuqina kakhulu kunokutshabalalisa i-gasket okanye kubangele ukuba ibhotile iqhekeke;
• Ukuhlolwa rhoqo kwenaliti yenkqubo yokutya: inaliti egugileyo okanye ekhubazekileyo inokuthintela i-gasket ekuzivaleni ngokwayo, nto leyo ebangela ukuvuza;
• Useto lobushushu olufanelekileyo: akufuneki idlule umda ophezulu wokumelana nobushushu be-gasket okanye isiciko, ngokubanzi ilawulwa kuluhlu lwe-110-130 ℃ ikhuselekile.

3. Iingcebiso zokucoca nokugcina iibhotile

Ukuze kusetyenziswe kwakhona iibhotile ezinokuba negalelo kwinqanaba lolawulo lweendleko okanye lophuhliso lweendlela, kufuneka kuqwalaselwe ngokukodwa iindlela zokucoca kunye nokugcina ukuze kuthintelwe ukungeniswa kokungcola okanye izinyibilikisi eziseleyo:

• Amanyathelo okucoca acetyiswayo: hlambulula izihlandlo ezininzi ngamanzi acocekileyo; hlambulula ngezinyibilikisi ezifanelekileyo zendalo; ukucoca nge-ultrasound kuxhomekeke kwinqanaba longcoliseko; ukomisa ngobushushu obuphezulu kwi-105℃-120℃ ukuqinisekisa ukuba akukho manzi okanye isinyibilikisi esiseleyo.
• Iingcebiso zokugcina: indawo yokugcina ecocekileyo, eyomileyo nevaliweyo, ukuthintela uthuli, izinto eziguquguqukayo zingaphinde zingcolise; ngaphambi kokusetyenziswa ukuba zigcinwe ixesha elide, kucetyiswa ukuba uphinde uhlole kwaye ucoce kwakhona; kuthintele ukuvezwa lilanga ixesha elide okanye kubushushu obuphezulu, ukuthintela ukonakala kokuguga kweglasi okanye i-gasket.

Ngokuziqonda ezi nkcukacha zibalulekileyo zokusebenza, awunakuphucula kuphela ukuchaneka nokuphindaphinda kovavanyo, kodwa ukwandise ngokufanelekileyo ubomi benkonzo yezixhobo kwaye unciphise izinga lokungaphumeleli. Kwizinto zohlalutyo ezifana nezinyibilikisi ezisele, ezibuthathaka kakhulu kwiinguqu zokulandelela, ulawulo oluneenkcukacha lwekhonkco ngalinye lokusebenza akufuneki lujongwe.

Isiphelo

Kwicandelo elilawulwa kakhulu nelichanekileyo lohlalutyo lwe-solvent yeentsalela zamayeza, i-headspace vial, nangona incinci, idlala indima ebalulekileyo nebalulekileyo. Ukususela ekugcineni, ukuvala kunye nokufudumeza isampuli, ukuya kulungelelaniso nenkqubo ye-autosampling, ngumgca wokuqala wokhuselo kuyo yonke ikhonkco yohlalutyo ukuqinisekisa ukuba idatha iyasebenza.

Iibhotile zentloko ezisemgangathweni azigcini nje ngokukhusela ukuthembeka kwesampuli, zithintele ukulahleka kwe-volatilization, kwaye ziphucule ukuhambelana kwenaliti, kodwa zikwasisiseko esifunekayo sokufunyanwa okuphindaphindwayo nokunobuthathaka kakhulu kuhlalutyo oluzenzekelayo. Ingakumbi xa kujongwana nohlalutyo lobungakanani benqanaba lokulandelela olufunekayo ngokwemigangatho ye-pharmacopoeia, isiphene esincinci sesiciko, izinto ezingafanelekanga, okanye umsebenzi wokuzalisa isampuli ongafanelekanga uya kuba nempembelelo engabonakaliyo kwiziphumo zohlalutyo.

Njengoko uphuhliso lwamayeza kunye nolawulo lomgangatho luqhubeka nokunyusa izinga lokuzenzekelayo kunye nokufunyanwa, imigangatho yomgangatho wee-headspace vials nayo iyaphakanyiswa. Ukusuka kubunyulu bezinto, ukuhambelana kwegama ukuya kukuhambelana kwenkqubo, ii-headspace vials zexesha elizayo akufuneki zihlale zizinzile kwaye zithembeke kuphela, kodwa zidlale indima "yojongano olusemgangathweni" kwilabhoratri yokucwangcisa, inceda ukulandelelwa kwedatha, ukuveliswa kwakhona kwendlela kunye nokuphuculwa ngakumbi kolawulo lomgangatho.