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Technical developments
of residue analysis
Technical developments of residue analysis
Johannes Jaschik
14/02/2020
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Residue analysis
2Technical developments of residue analysis
REGULATION (EC) No 1107/2009
Non visible !
We looking for residues (mainlyactive substances or metabolites) ofpesticides in products for which weexpect no use of these pesticides.
That means although we doing residue analysis - in mostcases we analysing contaminants in the given product.
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Residue analysis
There is no analytical possibility to distinguish whether the
substance detected was used on the product or originates
from a contamination.
3Technical developments of residue analysis
For residue analyis often either GC- and/or LC-MS/MS detection is used
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Approach of Residue analysis
4Technical developments of residue analysis
Evaluation based on a residue analysis for a productdepends on the scope and the sensitivity of theanalytical method(s).
Is it possible to check for all residues in foodstuff?
Free of pesticide residues?
Although this may be correct it can not be provencompletely.
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Analytical strategy for pesticides
How can pesticides be detected?
Multi method II(a few years ago)
Pesticides sold/used todayPesticides sold/used in the past
G
G
G
Technical developments of residue analysis 5
G
SingleMethods(e.g. Bromid)
Group methods
Multi method I(a few years ago)
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Analytical strategy for pesticides
How can pesticides be detected?
Multi method I(today)
Pesticides sold/used todayPesticides sold/used in the past
G
G
G
Technical developments of residue analysis 6
G
So even using always a multi method for analysis
limits findings to the scope of the multi method.
Multi method II(today)
Group methods
SingleMethods(e.g. Bromid)
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Scope of analysis (lab)
7Technical developments of residue analysis
How is this list created?
• Historical development
• Data from customers
• Information on legal developments
• Admission in countries of origin
• Specific for certain products
(experience)
• Practically/technically feasible
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Development multi method: possibilities
Scope changed over the time. In general getting broader, covering
more substances and furthermore getting more sensitive.
8Technical developments of residue analysis
• New analytical measurementssystems (LC-MS/MS)
• Better, more senstivemeasurement options
• New sample extractionmethods (e.g. Quechers)
• Better software solutions• Information about new
substances• Availability of reference
materiale.g. Fipronil RL
dropped to a few ppb
within the multi method
Reasons: e.g. MRL lowered for Fipronil
Scope
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Single methods (Glyphosate)
For single methods development is similar
9Technical developments of residue analysis
Glyphosate(RL: 0.1 mg/kg)
Glyphosate, AMPA,
Glufosinate(RL: 0.001
- 0.01 mg/kg)
Reason: pressure form organic products !
New method -new validation
New analytical measurements systems (LC-MS/MS)
Better, more senstive measurement options
New sample preparation methods (e.g. derivatisation)
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Single Methods (Phosphonic acid)
Because of the requirement to achieve an RL for
phosphonic acid 0.01 mg/kg a separate method was
developed.
10Technical developments of residue analysis
Fosetyl(RL: 0.01 mg/kg)Phosphonic acid(RL: 0.1 mg/kg)
Phosphonic acid,(RL: 0.01 –0.05 mg/kg)
New method
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Driver for development
As many pesticides as possible, at
the level of limit values.
11Technical developments of residue analysis
Pesticides not mentioned regulated with MRL 0.01 mg/kg
EU Regulation 396/2005 for pesticide residues in food
International Federation of
Organic Agriculture Movements
Action level / Orientation value
for pesticides:0.01 mg/kg
Why analysis?
Food safety / Knowledge (Fraud)!
In a few cases MRL evenlower than 0.01 mg/kg.
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Multi method
Reporting levels, always more sensitive, always better, all at the
same level?
What is a multi method?
Always a compromise:
12Technical developments of residue analysis
Due to the different
chemical properties,
these substances can be
determined individually,
but not all equally good.
• Broad scope• Maximum number of substances in
one analytical run• Robust• Reliable• Fast• … and of course cost-effective
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5 10 15Time, min
0.0
2.0e5
4.0e5
6.0e5
8.0e5
Chromatogram with 52 pesticides at the same level (1 mg/kg)
Multi method (LC-MS/MS)
Desmediphamhas the lowest
sensitivity
5 10Time, min
0
500
1000
1500
2000
2500
3000
Pirimicarbhas the highest
sensitivity
Exp. Val. Ratio: 3.00 RT Window: 30.0 sec
10Time, min
0.0
1.0e5
2.0e5
3.0e5
4.0e5
5.0e5
6.0e5
7.0e5
8.0e5
Intensity, cps
Technical developments of residue analysis 13
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Why not low RLs at ppb for all?
14Technical developments of residue analysis
Multi
method
costs, time, efficiency
Analysis of organic products: Besides food safety -
Identify food fraud or avoidable contamination
Technical limits toenlarge the scopeor improvesensitivity
Is contamination at very lowlevel avoidable?
Is an analytical result at a verylow level helpful for indication?
special singlemethod
new multi method
new equipment
Solutions?
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15Technical developments of residue analysis
Although residue analysis give an (important) indication
of the current residue situation in a given product –
for an evaluation of an organic product it is
neccessary to get an overview about the
whole picture of your product to draw
the right conclusions
(and take approbiate actions).
Final note
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16
Thank you very much!
Johannes Jaschik
Analytical Service Manager
Fon: +49-(0)40-881 448-452
www.eurofins.de
Johannes Jaschik
Analytical Service Manager
Fon: +49-(0)40-881 448-452
www.eurofins.de
?
Technical developments of residue analysis