Professional Documents
Culture Documents
SPECTROMETER
(ICP-MS)
29-09-2012
OVERVIEW
• INTRODUCTION
• INSTRUMENTATION
• PRINCIPLE
Sample introduction
Ion source
Mass analysers
Detection unit
Peak measurement
Methods of quantitation
Interferences
• PHARMACEUTICAL APPLICATIONS
• NEXT GENERATION OF ICP-MS
• CONCLUSIONS
INTRODUCTION
What is ICP-MS?
Inductively Coupled Plasma Mass Spectrometry
ICP-MS can:
• measure almost any element at ppt to ppm levels in almost any material.
• measure all elements in a single analysis.
• distinguish different element species (speciation).
• high sensitivity
• good matrix tolerance
• low levels of interferences
• ease of coupling to speciation techniques ( LA, LC and maybe GC)
INSTRUMENTATION
2 METALLIC CONES (SAMPLER AND
SKIMMER CONE ( 0.6-1.2mm ORIFICE, AT
760 TORR) TO SEPARATE FINE DROPLETS
(1-2%)FROM LARGER ONES
USING PERISTALTIC
PUMP(1ml/min)
750-1500W
PRINCIPLE
• Incoming ion draw an electron from the ground to neutralize the positive
charge of the incoming ion.
• A voltage is measured.
3.MULTIPLE COLLECTOR DEVICES
MEASUREMENT VARIABLES:
• Quantitative analysis
• Semiquantitative routine
• Isotope dilution
• Isotope ratio
• Internal standardization
INTERFERENCES
• Polyatomic Interferences
Minimized by:
1. Optimization of nebulizer gas flow (1.5-1.8ml/min).
2. RF power adjustment (500-800W).
3. Sampling position within plasma.
• Isobaric Interferences
Minimized by:
1. cold plasma technique
2. collision/reaction cell
3. High resolution mass analysers as double focussing magnetic field sector.
• Matrix Interferences
Minimized by: use internal standardization
ICP-MS : FIELDS OF APPLICATIONS
FIELDS OF APPLICATIONS
• Coupling techniques:
Chromatographic system
Laser ablation
LC-ICP-MS
Procedure:
• Laser beam focused onto sample surface in ablation
chamber or cell.
• Miniature plasma above sample ablates material from
surface.
• Resultant particulate material is transported to ICP-MS
with carrier gas stream (e.g. Ar)
• Sample is decomposed, atomised and ionized in ICP
plasma and analyzed in mass spectrometer.
• Clinical trials:
Simple metal analysis for active component confirmation
Monitoring of the metabolites of an administered drug
• Metal impurities – Leachables from pharmaceutical packaging materials
2. These components may be toxic or affect the stability of the drug product