際際滷

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Princip i izvedba tekuinske
kromatografije-masene
spektrometrije (LC-MS)
Tekua kromatografija - masena spektrometrija (LC-MS)
 Tehnika analitike kemije koja kombinira fizike mogunosti razdvajanja
tekuinske kromatografije (LC) sa sposobnostima masene analize masene
spektrometrije (MS)
 uvedenih 1980-ih godina
 mo転e se mjeriti u jednom analitikom postupku ^ ^ vrlo visoko osjetljiva i
selektivna
 korisna u mnogim aplikacijama
Komponente
Tekua
kromatografija
Ion izvor
Analizator
mase
Detektor
Tekua kromatografija
a) ulazni filter otapala, (b) crpka, (c) inline filtar otapala, (d) ventil za ubrizgavanje,
(e) predkolonski filtar, (f) stup, (g) detektor, (h) snima, (i) regulator protutlaka , (j)
spremnik otpada
Masena spektrometrija
Ion izvor
Analizator
mase
Detektor
PHOTO Dario
Masena spektrometrija
Jedinica za
ubrizgavanje uzorka
Ionizacija
Izvor
Analizator mase
Sustav detektora
Sustav podataka
Ionska generacija
Analiza podataka
Razvrstavanje iona prema masi (m / z)
Otkrivanje
 Krutina
 tekui
 pare
Ionizacija i suelje
Elektrosprejna ionizacija (ESI)
Kemijska ionizacija atmosferskog tlaka (APCI).
Atmospheric Pressure Photo-ionisation (APPI)
Termosprejna ionizacija(TSI)
Ionizacija zrake estica (PBI)
Ionizacija i suelje
Elektrosprejna
ionizacija
(ESI)
Ionizacija i suelje
Foto-ionizacija
atmosferskog tlaka
Kemijska ionizacija
atmosferskog tlaka
(APCI)
Ionizacija i suelje
Thermospray
ionizacija (TSI)
Ionizacija i suelje
Ionizacija estica zraka(PBI)
Analizatori mase
 Komponenta masenog
spektrometra
 uzima i odvaja ionizirane mase
na temelju omjera naboj i masa
 ih izlazi u detektor gdje se
detektira i kasnije pretvara u
digitalni izlaz.
Quadrupole
analizator
Vrijeme
analizatora
leta
Ionska
zamka
analizator
Hybrid
analizator
Analizatori mase
Quadrupole Analyzer
Time of Flight Analyzer
Ion Trap Analyzer
Analizatori mase
 Iona - elektriki otkrio detektor (su odvojeni prema omjer njihovih masa/naboj)
 Izbor detektor temelji se na:
 potrebno otkrivanje osjetljivosti i brzini
 Toplinska i kemijska postojanost
Detectors
Najmanje
osjetljiv
Faraday kup
detektor
1000 x veu
osjetljivost u
odnosu na
Faradaya kup
Fotomultiplikacij
skom detektor
Najosjetljiviji.
Koristi se za
visoke
rezolucije
Fotografski
detektor
Detektori
Faraday kup detektor
Detektori
Fotografski detektor
Detektori
Detektor fotomultiplikatora
Snimanje podataka
Snimanje potpunog masenog spektra - SCAN tehnika
Praenje odabranih iona - SIM tehnika
Praenje odabranih iona - SIM tehnika
Prijave Farmaceutska
analiza
Studije
biodostupnosti
Analiza produkta
razgradnje lijeka
Probir i
karakterizacija
potencijalnih
lijekova
Istra転ivanja
metabolizma
lijekova,
farmakokinetika
Identificiranje
ciljeva lijeka
Karakterizacija
biomolekula
Proteini i
peptidi
Oligonukleotidi
Forenzika
analiza
Analiza
okoli邸a
Pesticidi na hrani
Onei邸enje tla i
podzemnih voda

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32hr

Editor's Notes

  1. ESI operates according to the following scheme: 1) the column effluent from the LC containing analytes is pumped through a capillary which is held at high potential (2-6 kV) and nebulized. The applied voltage can be either positive or negative, depending on the analytes; nebulization is usually assisted pneumatically (except in nanospray); 2)the droplets that detach from a tip of the capillary contain an excess of positive or negative charge as a result of the applied high voltage; 3) electrical field gradient attracts charged droplets towards the entrance of the mass spectrometer; 4) charged analyte molecules are generated from the small charged droplets either by the charged residue model or by the ion evaporation model. Ion formation from the droplets is promoted by a flow ofdrying gas (usually heated nitrogen); 5) the ions, solvent vapor and drying gas molecules are sampled through a capillary into a first pumping stage (0.08-0.75 Torr) where they are supersonically expanded; 6)the ions and some other neutral molecules are sampled via a skimmer into the second pumping stage (0.001-0.01 Torr) containing an ion focusing and transfer device (usually RF hexapole or octapole and a set of lenses); 7)ions enter mass analyzer region (< 10-5 Torr).
  2. ESI operates according to the following scheme: 1) the column effluent from the LC containing analytes is pumped through a capillary which is held at high potential (2-6 kV) and nebulized. The applied voltage can be either positive or negative, depending on the analytes; nebulization is usually assisted pneumatically (except in nanospray); 2)the droplets that detach from a tip of the capillary contain an excess of positive or negative charge as a result of the applied high voltage; 3) electrical field gradient attracts charged droplets towards the entrance of the mass spectrometer; 4) charged analyte molecules are generated from the small charged droplets either by the charged residue model or by the ion evaporation model. Ion formation from the droplets is promoted by a flow ofdrying gas (usually heated nitrogen); 5) the ions, solvent vapor and drying gas molecules are sampled through a capillary into a first pumping stage (0.08-0.75 Torr) where they are supersonically expanded; 6)the ions and some other neutral molecules are sampled via a skimmer into the second pumping stage (0.001-0.01 Torr) containing an ion focusing and transfer device (usually RF hexapole or octapole and a set of lenses); 7)ions enter mass analyzer region (< 10-5 Torr).