Intshayelelo

Kwinkqubo yokuvelisa amayeza, i-solvents isetyenziswa ngokubanzi kwiinkalo ezininzi ze-API synthesis, ukukhutshwa, ukuhlanjululwa kunye neenkqubo zokuqulunqa. Nangona kunjalo, ukuba ezi zinyibilikisi zendalo azisuswanga ngokupheleleyo kwimveliso yokugqibela, "izinyibilikisi eziseleyo" ziya kwenziwa. Ezinye i-solvents zinetyhefu, i-carcinogenicity okanye ezinye iingozi zempilo ezinokuthi zibe khona, ngoko ke, ulawulo oluqinileyo lomxholo we-solvents eseleyo kwi-pharmaceuticals ayilona nje ikhonkco eliphambili lokuqinisekisa ukhuseleko lwamayeza ezigulane, kodwa kunye nenxalenye ebalulekileyo yolawulo lomgangatho wamachiza.

Kuhlalutyo lwe-headspace, isampuli ivalwe kwisitya esithile sokufudumeza, ukwenzela ukuba amacandelo aguquguqukayo akhululwe kwisithuba segesi ngaphezu kwesitya, kwaye ke le gesi ifakwe kwi-chromatograph yegesi ukuze ihlaziywe. Ukuthembeka kunye nokuchaneka kwesi sinyathelo esibonakala silula kuxhomekeke kakhulu kwi-key consumable - ii-vials ze-headpace.

Amagqabantshintshi eNdlela zokuHlalutywa kweNyibililo yokunyibilika

Uluhlu olubanzi lwezinyibilikisi ezishiyekileyo ezinokuthi zibekho kumayeza, aneempawu ezinobungozi ezahlukeneyo, kufuneka zibekwe ngokweendidi kwaye zilawulwe ngokweengozi ezinokuthi zibekho xa zihlalutywa kwaye zilawulwe. Izikhumbuzi zokuhlela eziphononongwe ngoontanga bamazwe ngamazwe zihlela izinyibilikisi ezishiyekileyo ngokwezi ndidi zintathu zilandelayo:

1. Iklasi 1: I-solvents engavumelekanga

Kubandakanya i-benzene, i-methylene chloride, i-1,2-dichloroethane, i-carbon tetrachloride, njl., ene-carcinogenicity enamandla kunye nobungozi bokusingqongileyo, kufuneka igwenywe kwinkqubo yokuvelisa. Imida ilawulwa ngokungqongqo kakhulu kwaye idla ngokubalwa kumanqanaba e-ppm okanye nangaphantsi.

2. Udidi 2: Izinyibilikisi eziphantsi kolawulo olulinganiselweyo

Kubandakanya i-toluene, i-acetonitrile, i-DMF, i-isopropyl alcohol kunye nokunye. Ubudala bezi zinyibilikisi zamkelekile phantsi kwemida ethile, kodwa basenayo imingcipheko yetyhefu ethile. Imida imiselwe ngokusekelwe kwi-ADI kwaye ngokuqhelekileyo ifuna ukubeka iliso elingqongqo.

3. Iklasi 3: Izinyibilikisi ezinobuthi obuphantsi

Ezi ziquka i-ethanol, i-propanol, i-ethyl acetate, njl., ezinetyhefu ephantsi kubantu kwaye ngokuqhelekileyo zibhekwa njengekhuselekile kumachiza ukuya kwi-50 mg yemihla ngemihla.

Ukuze kuchongwe ngokuchanekileyo uhlobo kunye nomxholo wezi zinyibilikisi ezishiyekileyo, i-chromatography ye-gas (GC) okwangoku yeyona ndlela iphambili yohlalutyo, enenzuzo ebalulekileyo yobuntununtunu obuphezulu, ukusebenza kakuhle kokwahlulahlula, kunye nokusebenziseka kwiikhompawundi eziguquguqukayo, ezinokuhlangabezana neemfuno zohlalutyo lwe-solvent eseleyo ukuze kubonwe umkhondo.

Phakathi kweendlela zokutofa ezahlukeneyo zemeteorological chromatography, itekhnoloji yokutofa kwe-headspace isetyenziswa kakhulu ekubhaqweni kwezinyibilikisi ezishiyekileyo kumayeza. Itekhnoloji ngothando lwaloo sampuli itywinwe kwibhotile ye-headspace, ifudunyezwe kwiqondo lokushisa elifanelekileyo, i-solvent kwisampulu ye-volatilization kwisithuba segesi yebhotile, kwaye emva koko ukusuka kwindawo yokukhupha umthamo othile wegesi eqeshiswe kwi-GC ukuze uhlalutye.

Izinto eziluncedo kwi-headspace feeding ziquka:

• Isampulu eyehlisiwe yonyango lwangaphambili: akukho misebenzi ye-solvent eyinkimbinkimbi okanye i-dilution efunekayo kwaye iisampuli zinokufudumeza ngokuthe ngqo kwigumbi elitywiniweyo;
• Ukuphucula ukuzala kunye nokuzinza: ngokulawula ngokuchanekileyo ubushushu bokufudumala kunye nexesha, ukuguquguquka kwesampuli kuhambelana ngakumbi, ukunciphisa iimpazamo zokusebenza;
• Ukuphepha ukungcoliseka okanye umonakalo wekholomu: kuphela isahlulo segesi esingeniswa kwinkqubo ye-chromatography, eyanciphisa kakhulu ukuphazamiseka kwamacandelo angabonakaliyo kunye nekholomu kunye ne-detector.
• Ifanelekile uhlalutyo oluzenzekelayo: inkqubo yokutofa kwe-headspace inokudityaniswa ngokungenamthungo kwi-autosampler, ifanelekile kwiimfuno zokubona izinto eziphezulu.

Nangona kunjalo, isikhongozeli sesampulu esizinzile nesithembekileyo, i-vials ye-headspace, iyimfuneko kuhlalutyo olusebenzayo noluchanekileyo lwe-headspace, olungalawuli kuphela indlela yokuziphatha kunye nokutywinwa kwesampulu, kodwa ikwachaphazela ngqo iziphumo zohlalutyo lokugqibela.

Inkcazo kunye neziphumo zeeVials ze-Headspace

Kwindlela yokulinganisa i-headspace, ukufudumeza kunye nokuguquguquka kwesampulu kunye nenkqubo yokufumana indawo yegesi zombini zenzeke kwimibhobho ye-headspace efana nezikhongozeli ezingenamoya, nangona kubonakala kulula, kodwa ukuyila kunye nokusebenza kwe-headpace ye-headspace kunempembelelo eqinisekileyo ekuthembekeni kwayo yonke inkqubo yokuhlalutya.
Iibhotile ze-Headspace zizixa zesampulu ezenzelwe inaliti ye-headspace kwi-chromatography yegesi. Ulwakhiwo lwayo oluqhelekileyo lubandakanya ezi ndawo zilandelayo:

Ibhotile: ngokuqhelekileyo yenziwe ngeglasi ye-borosilicate ephezulu, enokumelana nokushisa okuphezulu kunye nokungangeni kweekhemikhali, efumaneka ngokuqhelekileyo kwi-10ml, 20ml, okanye imiqulu emikhulu;

Ukuvulwa kwebhotile/umsonto: ubukhulu becala ukuvulwa okuqhelekileyo kwe-20mm, okufanelekileyo kwii-caps ze-aluminium kunye neenkqubo ze-autosampling;

Cap: ngokuqhelekileyo icinezelwe ukusuka kwizinto ezihambelanayo ukuze kuqinisekiswe ukuqina kwebhotile;

Gasket: kukho i-PTFE kunye ne-silicone yokwakheka kwezinto ezidibeneyo, ezinokumelana nobushushu obuphezulu kunye nokungangeni kweekhemikhali, inokumelana neesampuli ze-puncture ezininzi ngaphandle kokuvuza.

Indima ephambili yebhotile ye-headspace kukubonelela ngeendawo ezivaliweyo, ezingenayo kunye nezilawulwayo, i-solvents eguquguqukayo kwisampuli phantsi kweemeko zokufudumeza yindlela oh ibhotile ngaphezu kwendawo yegesi, ukubunjwa kommeli wokulingana kwegesi ye-solvent concentration kwisampuli yasekuqaleni.

Ngokukodwa, indima yayo ibonakaliswa kule miba ilandelayo:

Isiqinisekiso sokutywinwa: ukutywinwa okulungileyo ukuqinisekisa ukuba isampuli kwinkqubo yokufudumala okanye yokuphumla rhoqo ayiyi kuba ngenxa yokuvuza kunye nokulahleka kwe-solvent;

Ukukhuselwa kwezinto ezingasebenziyo: izinto eziphezulu zeglasi kunye ne-gasket zithintela ukusabela kunye nesampuli okanye i-solvent, ukuphepha ukungeniswa kwezinto zobuxoki okanye ukuphazamiseka komqondiso;

Iimeko zevolumu rhoqo: iibhotile ezisemgangathweni zifaka isandla ekuzinzeni kwe-headspace kunye nokuveliswa kwakhona, ukuququzelela ubungakanani kunye nokuthelekisa iziphumo zohlalutyo.

Iibhotile ze-headspace ezingathandekiyo ezisetyenziswa kwisampulu yesithuba sentloko esizenzekelayo. Ukuhamba komsebenzi ngokuqhelekileyo kuba ngolu hlobo lulandelayo:

1. Isisombululo sesampuli songezwa kwi-vial ye-headspace kwaye itywinwe;
2. I-autosampler yondla i-vial kwimodyuli yokufudumeza kwe-thermostatic;
3. Isampuli ishushu kwi-vial kwiqondo lokushisa elimiselweyo kwaye izakhi eziguquguqukayo zifudukela kwi-headpace;
4. Inaliti yokutofa igqobhoza i-gasket kwaye itsale umthamo wegesi kwi-headpace;
5. Irhasi yondliwa kwi-chromatograph yegesi yokwahlula i-alamu kunye nokufumanisa.

Kule nkqubo, ukuzinza kwesakhiwo, ukusebenza kwe-gasket puncture, kunye nokutywinwa kwee-vials ze-headspace zihambelana ngokuthe ngqo nokuhambelana kwesampuli kunye nokuchaneka kwemodeli. Ngokukodwa, ukusetyenziswa kwemigangatho, ethembekileyo ye-headspace vials ekusebenzeni okuzenzekelayo ngundoqo ekuqinisekiseni ukuba inkqubo yokuhlalutya iqhuba kakuhle kwaye inciphisa izinga lokungaphumeleli.

Kutheni i-Headspace Vials iyimfuneko?

Nangona i-chromatograph yegesi kunye ne-detector zizixhobo eziphambili kuhlalutyo lwe-solvent eshiyekileyo, indima ye-vial ye-headspace ibaluleke ngokulinganayo. Njengomthwali wabahlalutyi ukusuka kwisampulu yonyango lwangaphambili ukuya kwisitofu, ukusebenza kwayo kuhambelana ngokuthe ngqo nokuzinza kwenkqubo yohlalutyo kunye nokuthembeka kwedatha.

1. Isampula yemfezeko kunye nolawulo oluguquguqukayo

Amachiza okunyibilikisa ashiyekileyo abilisa kancinci, adityaniswe nezinto eziphilayo anokuchaphazeleka kakhulu ekulahlekeni ngexesha lokuvezwa, ukufudumeza okanye ukugcinwa. Ukuba i-vials ye-headpace ayigcinwanga kwisitywina esiqinileyo kulo lonke umjikelezo wokuhlalutya, umxholo we-solvent unokutshintsha, okukhokelela kwiziphumo ezichaseneyo.

Iibhotile ze-headspace ezisemgangathweni ziyakwazi ukufudumeza ngaphezu kwe-100-150 ° C kwisimo esitywiniweyo, ukuqinisekisa ukuba amacandelo aguquguqukayo akhululwa kuphela kwaye ahlalutywe phantsi kweemeko ezimiselweyo;

Ukulawulwa ngokuchanekileyo kwesampulu ukufikelela kwi-gas-liquili equilibrium kwiqondo lokushisa rhoqo kunye nomthamo wandisa ukuchaneka kunye nokuphindaphinda kweziphumo.

2. Impembelelo yokutywinwa kwentsebenzo kwiziphumo zohlalutyo

Inkqubo yokutywina ye-Vial ye-Headspace idla ngokuba namacandelo amathathu: i-cap, i-gasket kunye ne-mouthpiece. Ukutywinwa okungalunganga nakweyiphi na indawo kunokubangela ukuvuza kwesampulu, ingxolo ephezulu yangasemva, okanye ukungcoliseka kwesampulu.

Umgangatho ophezulu we-PTFE / i-silicone gaskets ayixhathisi kuphela ukushisa okuphezulu kunye neekhemikhali, kodwa inokumelana neepunctures ezininzi kwaye igcine isitywina esihle;

I-gasket yekhwalithi ephantsi okanye i-loose gland inokubangela ukuba i-solvent ibaleke ngaphambi kokuhlalutya okanye ngexesha lokufudumeza, ichaphazela ngokuthe ngqo indawo ephezulu kunye nokunciphisa ukuchaneka kobungakanani.

3. Ukuhambelana neenkqubo ze-autosampling

Izitofu ze-headspace ezizenzekelayo ziqhele ukusetyenziswa kwiilabhoratri zanamhlanje ukuphucula ukusebenza kakuhle kunye nokungaguquguquki kweziphumo, kwaye uyilo olusemgangathweni lwe-Headspace vial luvumela ukuba lulungelelaniswe ngokuthe ngqo kwiimpawu eziphambili zenkqubo yokutofa.

Imilinganiselo esemgangathweni iqinisekisa ukuba iibhotile ziyakwazi ukuchongwa ngokuzenzekelayo, zibekwe ngokuchanekileyo kwaye zihlatywe kwi-injector;

Ukunciphisa iimpazamo ezenziwa ngesandla kuphucula ukusebenza kwesampulu kunye nokuhambelana kwedatha, okwenza i-Vial ye-Headspace ilungele iimeko zokuvavanya okuphezulu.

4. I-inertness yekhemikhali yezinto

I-chemistry yeebhotile kunye nezixhobo zokutywina akufanele zihoywe xa kuhlalutywa i-solvents trace kunye. Izinto ezikumgangatho ophantsi zinokubhengeza okanye zisabele ngeemolekyuli ezinyibilikayo, ezikhokelela kwiziphumo ezicalu-calulo.

Iglasi ye-Borosilicate i-inert yekhemikhali kwaye i-thermal stable, ikhusela i-adsorption ye-solvent okanye ukuchithwa kwe-thermal;

Kwezinye iinkqubo ezikhethekileyo ze-solvent, ii-gaskets ezenziwe ngezinto ezikhethekileyo zifunekayo ukuze kuqinisekiswe uvakalelo lokubona kunye nokuzinza kwesampuli.

I-Vial ye-Headspace ingaphezulu nje kwesitya sesampuli esilula, siyinxalenye ephambili ekuqinisekiseni ukuba iziphumo zohlalutyo lwe-solvent olushiyekileyo luyinyani, aluguquguquki kwaye luyaphinda luvelise kwakhona. Ithatha imisebenzi emininzi ebalulekileyo kulo lonke ikhonkco lokuhlalutya, njengokhuseleko lokutywinwa, ukulawula ukuguquguquka, ukulinganisa inkqubo, isiqinisekiso sokungangeni kweekhemikhali, njl.

Izinto eziphambili ekukhetheni iVial ye-Headspace yasekunene

Kuhlalutyo lwe-solvent eshiyekileyo, ukukhethwa kwe-vial ye-headspace efanelekileyo yinto efunekayo ukuze kuqinisekiswe ukuchaneka kwedatha kunye nendlela yokuhambelana. Iimfuno ezahlukeneyo zovavanyo, iintlobo zesampulu kunye neeplatifti zesixhobo zineemfuno ezahlukeneyo zemathiriyeli ye-vial ye-headspace, ulwakhiwo kunye nokusebenza. Ezi zinto zilandelayo zibalulekileyo kufuneka ziqwalaselwe xa ukhetha i-vial ye-headspace:

1. Izinto eziphathekayo: uhlobo lweglasi kunye nokungafihli

• Iglasi yeklasi ye-borosilicate: into ekhethiweyo yebhotile yohlalutyo lwe-solvent eseleyo. Ukushisa kwayo okugqwesileyo kunye nokuchasana kweekhemikhali kunye nokugxininiswa okuphantsi kakhulu kwee-ion ezinqambileyo zithintela ukuphendula kweekhemikhali phakathi kwe-solvent kunye nebhotile, ukuphepha ukuchasana kobuxoki okanye ukuphazamiseka komqondiso.
• Ukucaca okuphezulu kwebhotile: ivumela ukujonga ngokukhawuleza isimo sesampulu ngexesha lokutshiza, ukuhlolwa okanye ukujonga umgangatho, njengobukho bemvula, inani elichanekileyo lolwelo, njl., kunye nokuchongwa lula ngeenkqubo ezizenzekelayo.

2. Ukukhetha umthamo: iinkcukacha ezisetyenziswa ngokuqhelekileyo 10ml, 20ml

Ukukhethwa komthamo weVial ye-Headspace kufuneka kusekwe kwindibaniselwano yezi zinto zilandelayo:

• Umthamo wesampuli: Ngokuqhelekileyo umthamo wesampuli malunga ne-50% yomthamo webhotile ukuqinisekisa indawo eyaneleyo yentloko (indawo yegesi) yokulinganisa ukulinganisa;
• IiMfuno zeNdlela yokuHlalutya: Ngokomzekelo, i-USP <467> i-residual solvent method incoma ukusetyenziswa kwe-20 ml ye-headspace vial;
• Ukuhambelana kwe-Autosampler: qinisekisa ukuba ibhotile ekhethiweyo isekela imodeli yesixhobo esisetyenzisiweyo, ngakumbi ibhotile ngaphezu kwe-aperture.

3. Uhlobo lwe-gasket yokugubungela: ukutywinwa kunye nokufaneleka kweekhemikhali

Izinto zeGasket: eyona isetyenziswa ngokuqhelekileyo yi-PTFE i-gasket edibeneyo, isakhiwo sayo se-double-layer sidibanisa i-inertia yekhemikhali ye-PTFE kunye ne-elasticity ye-silicone yokutywinwa, inokumelana nokushisa okuphezulu kunye nokugcina ukutywinwa okulungileyo; kwizinyibilikisi ezomeleleyo okanye ezomeleleyo, ungakhetha ucoceko oluphezulu lwe-PTFE umaleko wegasket eqinisiweyo.

Iintlobo zekepusi yebhotile: I-Aluminiyam i-caps ifanelekile kwizixhobo ezininzi, kunye ne-gland eqinile kunye nokutywinwa okugqwesileyo; Iminqwazi yemagnethi ifanelekile kwiinkqubo ze-autosampling kunye nokuchongwa kwamagnetic, okunceda ukuphucula ukusebenza kakuhle kokutya kunye nokuchaneka kokubeka; Iminqwazi enemisonto, ngelixa ilungele ukusebenza ngesandla, ayinakutywinwa kunye neentlobo zamadlala kwaye ifaneleke ngakumbi kwizigaba zophuhliso okanye iimeko ezingezizo eziphezulu.

4. Ukusetyenziswa kwakhona kunye nokuqwalaselwa kweendleko

Iibhotile zeglasi eziphinda zisebenziseke (ezifuna ukucocwa kobushushu obuphezulu kunye ne-sterilization) zifanelekile kwezinye iindlela ezingezizo i-pharmacopeial okanye izifundo zophuhliso kwaye zinokunciphisa iindleko zexesha elide;

Nangona kunjalo, kwimveliso ye-GMP okanye iilabhoratri zokulawula umgangatho osesikweni, ii-vials ezisetyenziselwa enye zingcono ukuqinisekisa ukucoceka kunye nokuphepha ukungcoliseka;

Xa kuthengwa ngeebhetshi, kukwabalulekile ukulinganisa umgangatho webrand, ibhetshi-to-batch ukungaguquguquki, kunye nexabiso lokukhetha umthengisi obonelela ngebhalansi yokusebenza kunye neendleko.

Ukhetho olunengqiqo lwe-vial ye-headspace alukho nje umsebenzi osisiseko, kodwa kunye nokubonakaliswa kokuqonda kokulawula umgangatho. Lonke ukhetho olubonakala luncinci lweparamitha ludlala indima ebalulekileyo ekuchanekeni kwesiphumo, ukuzinza kwenkqubo kunye nokusebenza kakuhle kwebhubhoratri. Ke ngoko, ukuqonda okunzulu kwezi zinto ziphambili sisakhono sobuchwephesha esibalulekileyo kuwo wonke amagcisa asebenza kuhlalutyo lwamayeza.

Imibuzo Ebuzwa Rhoqo kunye namanqaku

Nangona ii-vials ze-headspace zisetyenziswa ngokubanzi kuhlalutyo lwe-solvent eseleyo, uluhlu lweengxaki lusenokuthi luvele ekusebenzeni ngenxa yokuphatha okungafanelekanga okanye ukhetho lwezinto ezisetyenziswayo. Ezi zilandelayo ziingxaki eziqhelekileyo kunye neengcebiso zothintelo:

1. Ukuphepha njani ukungcoliseka kwesampulu

Ukungcoliswa komnqamlezo akuchaphazeli kuphela ukuchaneka kweziphumo zohlalutyo, kodwa kunokubangela ukuphazamiseka kwexesha elide elifihliweyo kunye nenkqubo yokufumanisa, ngakumbi kumngcipheko ophezulu xa uhlalutya amanqanaba aphantsi. La manyathelo alandelayo anokuthintela ngempumelelo le ngxaki:

• Beka phambili ukusetyenziswa kweevials ezilahlwayo kunye neecap pads: le yeyona ndlela ichanekileyo kunye neyona ndlela isebenzayo, ngakumbi kulawulo lomgangatho wamachiza kunye novavanyo lokulawula;
• Tshintsha okanye ucoce ngokucokisekileyo iingqayi eziphinde zasetyenziswa: ukuba ukusetyenziswa kwakhona kuyafuneka, qinisekisa ukuba zicocwe ngokucokisekileyo kusetyenziswa amanyathelo afana namanzi adiyiniweyo, izinyibilikisi eziphilayo, kunye nokomisa ubushushu obuphezulu;
• Iindlela ezingqongqo zokuhambisa: sebenzisa izixhobo zombhobho ezikhethekileyo ukunqanda ukuthontsiza kwesampulu okanye ukujikeleza ibhotile;
• Coca izixhobo zebhentshi eziphezulu kunye neiglavu: xa uphatha i-solvents eziguquguqukayo, iiglavu kufuneka zitshintshwe rhoqo ukuze zithintele ukusabalalisa ukungcola ngokuphatha.

2. Ukuvuza kweCap ngexesha lokufudumala

Kuhlalutyo lwe-headspace, isampuli kufuneka ifudunyezwe kwi-80-120 ° C okanye nangaphezulu. Ukuba i-caps okanye i-gaskets ayivalwanga ngokufanelekileyo, i-solvents inokubaleka ngexesha lenkqubo yokufudumeza, okubangela ukuguquguquka kwedatha okanye iziphumo eziphantsi.

• Khetha iigaskets ezikumgangatho ophezulu: kufuneka babe nokuxhathisa ubushushu kunye ne-puncture elasticity ukuqinisekisa ukuba itywina alikhululi;
• Amandla e-capping achanekileyo: i-manual okanye i-automatic capping ifuna ukumodareyitha, ikhululekile kakhulu inokuvuza, iqine kakhulu inokutshabalalisa i-gasket okanye ibangele ukuba ibhotile igqabhuke;
• Ukuhlolwa rhoqo kwenaliti yenkqubo yokutya: inaliti egugileyo okanye eyonakeleyo inokuthintela i-gasket ukuba ingazitywini ngokwayo, ibangele ukuvuza;
• Ukumiselwa kobushushu obufanelekileyo: akufanele idlule umda ophezulu wokumelana nobushushu be-gasket okanye i-cap, elawulwa ngokubanzi kuluhlu lwe-110-130 ℃ ikhuselekile.

3. Iingcebiso zokucoca i-Vial kunye nokugcinwa

Ukusetyenziswa kwakhona kwe-vial enokuthi ibandakanyeke kulawulo lweendleko okanye kwisigaba sophuhliso lwendlela, ingqwalasela ekhethekileyo kufuneka ihlawulwe ekucoceni nasekugcinweni kweendlela zokuthintela ukuqaliswa kokungcola okanye i-solvents eseleyo:

• Amanyathelo okucoca acetyiswayo: hlambulula amaxesha amaninzi ngamanzi adibeneyo; hlambulula ngezinyibilikisi ezifanelekileyo; ukucocwa kwe-ultrasonic kuxhomekeke kwinqanaba lokungcola; ubushushu obuphezulu bomisa kwi-105℃-120℃ ukuqinisekisa ukuba akukho kufuma okushiyekileyo okanye isinyibilikisi.
• Iingcebiso zokugcina: ukugcinwa okucocekileyo, okomileyo kunye nokutywinwa, ukuphepha uthuli, izinto eziguquguqukayo ziphinde zingcoliseke; ngaphambi kokusetyenziswa ukuba igcinwe ixesha elide, kuyacetyiswa ukuba uphinde uhlolisise kwaye uhlambulule kwakhona; kunqande ukuvezwa kwexesha elide kukukhanya kwelanga okanye ubushushu obuphezulu, ukuthintela ukuwohloka kweglasi okanye ukuguga kwe-gasket.

Ngokulawula ezi nkcukacha zibalulekileyo zokusebenza, awukwazi nje ukuphucula ukuchaneka kunye nokuphindaphinda kovavanyo, kodwa ukwandise ngokufanelekileyo ubomi benkonzo yezixhobo kunye nokunciphisa izinga lokungaphumeleli. Kwizinto ezihlalutyayo ezifana nezinyibilikisi ezishiyekileyo, ezinobuthathaka kakhulu ekulandeleni iinguqu, ulawulo olucacileyo lwekhonkco ngalinye lokusebenza akufanele lihoywe.

Ukuqukumbela

Kwinkalo elawulwa kakhulu kunye nechanekileyo yohlalutyo lwe-solvent yeentsalela zamachiza, i-vial ye-headspace, nangona incinci, idlala indima ebalulekileyo kwaye ibalulekile. Ukususela ekugcinweni, ukutywinwa kunye nokufudumeza isampuli, ukulungelelaniswa nenkqubo ye-autosampling, ngumgca wokuqala wokukhusela kulo lonke ikhonkco lokuhlalutya ukuqinisekisa ukuqinisekiswa kwedatha.

Iibhotile ze-headspace ezisemgangathweni azigcini kuphela ukunyaniseka kwesampulu, ukuthintela ilahleko ye-volatilization, kunye nokuphucula ukuhambelana kwenaliti, kodwa zisisiseko esiyimfuneko sokuveliswa kwakhona kunye nokufunyanwa okubuhlungu kuhlalutyo oluzenzekelayo. Ngokukodwa xa ujongana nenqanaba lokulandela uhlalutyo lobungakanani obufunwa yimigangatho ye-pharmacopoeia, i-cap defect encinci, izinto ezingafanelekanga, okanye isampuli engafanelekanga yokuzaliswa kwesampula iya kuba nefuthe elingenakulinganiswa kwiziphumo zohlalutyo.

Njengoko uphuhliso lweziyobisi kunye nolawulo lomgangatho luqhubeka nokwandisa iqondo lokuzenzekelayo kunye nokufumanisa i-throughput, imigangatho yomgangatho wee-vials ze-headspace nayo iyaphakanyiswa. Ukususela ekuhlambulukeni kwezinto eziphathekayo, ukuhambelana kwegama ukuhambelana kwenkqubo, iibhotile ze-headspace zexesha elizayo akufanele zizinzile kwaye zithembeke kuphela, kodwa ziphinde zidlale indima "ye-interface esemgangathweni" kwi-laboratory yokucwangcisa, ukunceda ukulandelwa kwedatha, ukuveliswa kwendlela kunye nokuphucula ngakumbi ulawulo lomgangatho.