analytical methods, and analytical tehnics in food and
TRANSCRIPT
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Analytical methods, and analytical tehnics in food and environmental monitoring
WP 2
Saša Popov (ESV)
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Analysis of food and environmental samples -classification by analytical techniques:
-instrumental analysis;-non-instrumental analysis-standard analytical methods (gravimetriy, volumetry, senzory....);
Instrumental analysis classification:
- Spectrometric (UV-VIS, IR, FTIR, AAS, ICP-OES,...);- Chromatografic (gas chromatography, liquid chromatography, TLC,...);- Electroanalytical methods (potenciometry, voltametry, conductometry,...)- Others (MS, MS/MS, NMR, Coupled tehniques (GC/MS, GC/MSMS, LC/MS, LC/MSMS,...));
All kinds of listed techniques are used to better define the product performance!
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Some tehniques in Enological station Vršac
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Nature of sample characteristics (food safety and environment):
- Quality of sample – composition of sample (proteins, fats, sugars, acids, macroelements, microelements....);
- Contaminants-health safety (heavy metals, pesticides, mycotoxins, PAHs, PCBs, antibiotics, dioxins, phenols....);
- microbiological profile ;
Modern science and analytics today, attaches increasing importance of contaminants in food and environmental samples!
contaminants instrumental analytical tehnics
connected
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Determination of pesticide contaminants in fruits and vegetables
- QueChers method of sample preparation
(10 g sample + 10 ml ACN + ISTD + QuEChERS tube), extraction, cleaning, centrifugation, optional evaporation;
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Finished sample preparation
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- Analysis by GC / MSD
(injection (liquid), separation on chromatographyc column (HP5-MS), jonization (EI), detection (MS));
Analysis over 100 active components of pesticides (organochlorines, organophosphates, pyrethrins, triazines, others);
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Possible problems - errors:
Losses in sample preparation
- strictly use the ISTD during the preparation (PCB 52, Triphenyl phosphate,...);
- quantitatively transferr extracts and carefully evaporate;
Influence of matrix
- additional sample cleaning;
- LLE (with hexane/20% NaCl (w/w) mixture) leads to significant reduction of matrix co-extracts ;
- select different Qualyfiers which you record with MSD;
Confirmation some active component
- spike sample;
- additional sample concentration;
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Scan chromatogram of mentha piperita
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comparation of MS spectra chlorpyrifos from sample and library of MS spectra
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SIM chromatogram of mentha piperita
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SIM chromatogram of spiked mentha piperita
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SIM chromatogram of mentha piperita
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Determination of metals in water, soil and sludge samples by ICP-OES(US EPA 200.7)
Sample preparation:-Microwawe digestion, filtration, evaporation, dilution;
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ICP-OES determination:
- conditions settings;
- calibration;
- ICP-OES determination;
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Possible problems - errors:
- Bad sample preparation (losses, low preparation temperature, contamination, ...);
- Influence of matrix (bad choice of characteristic emission lines,...);
- Bad conditions on ICP-OES (spectral shift of the characteristic lines, not using of ISTD,...)
WHAT CAN WE DO?
- Analysis of CRM-corection of sample preparation and ICP-OES determination;
- Check and set conditions on ICP-OES (the optics with special standards solution, choice of different emission lines, speed of sample uptakes, ....;
- Spike samples;
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Example of bad determination on ICP-OESsoil samples– determination of CEC
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Example of good determination on ICP-OESsoil samples– determination of CEC
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Example of influence ISTD on ICP-OES determinationsoil samples
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Effect of stability on ICP-OES determination of CRM sample (strawberry leaves)
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Effect of stability on ICP-OES determinations of CRM sample (strawberry leaves) –power failure
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FOR SUCCESSFUL ANALYSIS
you must know, look, think, feel and do analytics