Tendințe recente în analiza cromatografiei lichide-spectrometrie de masă

a contaminanților organici în probele de mediu

Mira Petrovic, Marinella Farré, Miren Lopez de Alda, Sandra Perez, Cristina Postigo,
Marianne Köck, Jelena Radjenovic, Merixell Gros, Damia Barcelo
 Ce invatam din acest articol?

De ce LC-MS?

Prepararea probei pentru

LC-MS
Metode imbunatatite de
LC
Advances in chromatographic
separation
Analiza LC-MS a
pesticidelor polare

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De ce LC-MS? Ce se determina?

Determinarea urmelor cu feptograme 1*10

Algal
-13g and cyanobacterial toxins

Plaja larga de determinare Drugs of abuse

Sampling mai usor Organometallics
Nanomaterials
Posibilitatea automatizarii
Timp de analiza mai mica Polar pesticides
Surfactants
Pharmaceuticals
Hormones

Metoda clasica, probleme:
• Exhaustive extraction-Large number of
matrix components
• Sample pretreatmens-time and labor c
onsuming
• Tedious extraction and clean-up protoc
ols- 75% of analysis time
• High number of samples-problem
Prepararea probelor
Remediere:
• Devolepment of Cost effective sample
handling techniques characterized by t
he efficiency and simplicity of operation
s and devices
Solutie:
• Automation through coupling of sample prep
aration units and detection systems(SPE-LC)
• Integration of several sample preparation ste
ps into one
• Application of tailored sorbents
 Automated instruments
On-line sample extraction coupled to LC-MS
Using different extraction supports or sorbents such as:
• Disposable cartridge
• Restricted access materials
• Monolithic materials
Tailoring extraction and clean-up materials:
• Molecularly imprinted polymers- high potential for single gro
up analysis, due to molecular recognision - determination of d
iclofenac, acidic pharmaceuticals, halogenated derivatives
Carbon nanostructures
• Carbon nanotubes- as sorbent materials sin SPE- extraction of
chlorophenols ad pesticides
 Passive samplers
• Long term monitoring- large number of samples taken from sampling poi
nt aver the monitoring time-probem!
• Solution- combination into a single step of sampling, analyte isolation an
d preconcentration- they are used to measure time averaged water concent
ration.
Membrane-based samplers – for non-polar lipophilic compunds
• Semi-permeable membrane devices
• Solvent-filled and sorbent-filled devices

Advantages of SPE
• Variety of sorbents available
• Faster
• Posibility of automation
 Advances in chromatographic separation
Reducing the column particle diameter- increase speed and efficiency

Application of hydrophilic interaction chromatography- for the separation

of polar compounds( pharma and metabolites)
 LC-MS analysis of polar pesticides
• The use of MS detection allows analysis without complete
chromatographic separation between the analytes- shorte
ning of the chromatographic run time
• Pesticide transformation products- time-of-Flight analyses(
TOF)- ion scan mode- Ions are accelerated by an electric f
ield of known strength. This acceleration results in an ion
having the same kinetic energy as any other ion that has t
he same charge