Particle Engineering via Sonocrystallization: The Aqueous ...
An evaluation of a particle beam interface at high aqueous ...
Transcript of An evaluation of a particle beam interface at high aqueous ...
An Evaluation of a ParticleBeam Interface at High
Aqueous Concentrations
Jennifer M. Duker and Thomas C. Marecic
Problem...
Reverse phase HPLC can typically include highaqueous solvent conditions.
MS is becoming a preferred detection device forHPLC.
Compatibility between the two techniques ischallenging.
Stages of Particle Beam LC/MS
HPLC INTERFACE MASSDETECTOR
Phase Momentum
LC Separate Separate MSLiquid _ "- "- _ GasPhase Phase
INTERFAC
Phase Momentum
Separate Separate
Aerosol Enrichment/generation Pressure
ReductionDesolvation
Phase Separation
GoalTo separate the solvent from thesolute by converting the solvent tothe gas phase and the solute t°particles
° Nebulization - generation of anaerosol
° Desolvation - separation of thesolvent from the solute
Momentum Separation
,-GoalTo remove gas phase whiletransporting particles into MS
° Effective removal of solvent• Enrichment of solute
INTERFACE
Phase Momentum
Separate Separate
Aerosol Enrichment/generation Pressure
ReductionDesolvation
Why are some solvent conditionsmore difficult?
Solvent B.Pt.
ProticWater 100 10.5Methanol 64.7 8.9
AproticAcetonitrile 81.6 7.8THF 66.0 7.6
Phase Separation(Cpdt)g+(Cpdt)soI
(Cpdt)l AHvap
TOcmeasured iDEAL
Power (watts)
100% Solvent Evaporation0% Solute Evaporation
Summary of Phase SeparationTM
ThermaBeam
Thermal/Pneumatic NebulizationDesolvation
Analysis of Environmental CompoundsExperimental Conditions
Analytical ConditionsCompounds: caffeine
methomylbenzidine
Column: Waters Nova-Pak C18 (2.0 x 150 mm)Mobile Phases: (1)72:28 ammonium acetate:ACN
(2)87:13 ammonium acetate:ACNFlow rate: 250 uL/min
MS Review
Ivent Conditions72:28
NH4OAc:ACN
MaxplotChromatogram
100 to 200 amu
PDA Review
Fi p
HighAqueousSolvent
Conditions87:13
NH OAc:ACN4
MS Review
HighAqueousSolvent
Conditions87:13
NH4OAc:ACN
View Cube
3D
Chromatogram
TICContour View
MaxplotChromatogram
Maxplot Chromatogram100 to 200 amu
Environm
Overlay of Mass Spectra
_ra::_i!_!_ii_i__Hel:::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::
•Eile',"_!!i_'_i_!_E_ditl;ii__!_PlOt_D,C p
ExtractedMass
Spectrumof methomyl
__Hetp!!i
Extracta
Mass
Spectrumof
benzidine
ExtractedMass
Spectrumof benzidine
Extracta
Mass
Spectrumof
caffeine
ExtractedMass
Spectrumof caffeine
Conclusions
Analysis using high aqueoussolvent conditions is possible
,_ThermaBeam TM lessens the
challenge for compatibility betweenHPLC and MS
AutoOptimize adjusts the interfaceto handle high aqueous conditions