Pesticide Residue Analysis — EN 15662 QuEChERS / (EC) 396/2005

What Is Pesticides?

Pesticide residue analysis is the determination of pesticide residues in plant and animal foods. The common approach is the QuEChERS method defined in EN 15662: the sample is extracted with acetonitrile, phase separated by addition of salt, cleaned by dispersed solid phase extraction and hundreds of active substances are screened simultaneously in LC-MS/MS and GC-MS/MS.

Purpose of Pesticides

The aim is to demonstrate that residue levels comply with the maximum residue limits (MRL) under EC 396/2005. MRL non-compliance is one of the most common reasons for rejection in exports.

Which Products Is Pesticides Applied To?

Fresh fruit and vegetables
Cereals and pulses
Tea, spices and dried herbs
Baby food and children's foods
Animal products and feed

In Which Sectors Is Pesticides Used?

FoodAgricultureRetailAgricultureEnvironment

Standards Related to Pesticides

TS EN 15662 (QuEChERS — multi-residue method with LC-MS/MS and GC-MS/MS)
SANTE analytical quality control guide
TS EN 12393 series (high residue methods in non-oily foods)
TS EN 1528 series (pesticides and PCBs in oily foods)

Pesticides Conditions

Scope: The list of active ingredients to be screened is determined according to the target market and product.
Extraction: QuEChERS; acetonitrile extraction and distributed cleanup
Measurement: LC-MS/MS and GC-MS/MS together; One technique does not cover all active ingredients
Quality control: Recovery and matrix effect controls according to SANTE guidance

Equipment for Pesticides

LC-MS/MS
GC-MS/MS
QuEChERS extraction kits and centrifuge
Mill and homogenizer
Analytical balance

Sample Requirements for Pesticides

Sample representing the lot; The sampling method must comply with the legislation
A sufficient amount of sample (usually 1 kg or more)
Product, production region and target market must be declared
The sample must be delivered at the appropriate temperature and without delay.

Duration of Pesticides

Analysis takes several working days due to extraction, cleanup and two separate chromatographic measurements. Confirmation of positive findings requires additional time.

Pesticides Procedure

1The sample is taken and homogenized in accordance with the legislation.
2Acetonitrile extraction is performed using the QuEChERS method.
3Phase separation is achieved by adding salt.
4It is cleaned by dispersed solid phase extraction.
5Measurements are made with LC-MS/MS and GC-MS/MS.
6Findings are compared with MRL values.

Pesticides Acceptance Criteria

(EC) 396/2005 defines separate maximum residue limits (MRL) for each active ingredient and each product; In cases where no data is available, the default limit applies. Separate and stricter provisions apply to baby and young children's food. The MRLs to be applied are confirmed from current values in the EU pesticide database.

Evaluation of Results

The result is evaluated taking into account the measurement uncertainty; The SANTE guide describes how to perform this assessment. Additionally, an active substance that is not on the targeted screening list will not appear in the report: substances monitored by the target market must be included in the list.

Pesticides Report

Sample description, batch and sampling information
Number and list of active ingredients screened
Applied methods and measurement techniques
Detected residues, their concentrations and detection limits
Recovery and quality control results
Compared MRL values

Accreditation

EUROLAB holds internationally recognised accreditation obtained from accreditation bodies party to the IAF and ILAC multilateral recognition arrangements, under ISO/IEC 17025 for laboratory testing, ISO/IEC 17020 for inspection and surveillance, and ISO/IEC 17021-1 and ISO/IEC 17065 for system and product certification. This chain ensures the reports and certificates issued are accepted worldwide.

Whether this test can be offered within accredited scope depends on your product and the standard applied; since accreditation is method-based, the scope is confirmed in writing at the quotation stage.

Scope and authorisations

Related Regulations

Regulation (EC) 396/2005 on Maximum Limits of Pesticide Residues
(EU) 2016/127 (infant and follow-on formulas)
(EC) 178/2002 General Food Law

Food Testing — What Does This Testing Field Cover?

The section below describes the field that the Pesticides test belongs to; the conditions and acceptance criteria of this particular test are given in the sections above. The scope specific to your product is confirmed in writing at the quotation stage.

Food testing shows that a product is safe for consumption and contains what its label states. The family works along three axes: microbiological safety, chemical safety and nutritional composition. All three require different laboratory infrastructure, a different body of methods and a different turnaround time.

The most distinctive feature of the field is TIME PRESSURE. A steel specimen can wait on a shelf; a raw milk or fresh meat sample cannot. The time the sample was taken, the transport temperature and how long it takes to reach the laboratory directly determine the validity of the result. In food microbiology the cold chain record is therefore an inseparable part of the test report.

On the microbiological side there are two different questions and they must not be confused. DETECTION of a pathogen is a qualitative question: is Salmonella present in the sample or not? ENUMERATION of indicator organisms is a quantitative question and an indicator of production hygiene. The absence of a pathogen in a product does not show that hygiene is good; if the total mesophilic aerobic count is high, there is a problem in the process.

On the chemical side, pesticide residues, mycotoxins, heavy metals, additives, veterinary drug residues and process contaminants (acrylamide, furan, PAH) are measured. Multi-residue methods in this area (QuEChERS-based LC-MS/MS and GC-MS/MS) can screen hundreds of active substances in a single analysis; limits are defined separately for each product–substance pair.

On the composition side, protein, fat, moisture, ash, fibre, sugar profile, fatty acid composition, vitamin and mineral content are determined. These values are the basis of the nutrition declaration on the label and the tolerance ranges are defined in legislation — the difference between the declared value and the measured value must stay within that tolerance.

There is NO CE marking on food, and this shapes how the field works. Conformity is demonstrated through operating a HACCP-based food safety system, complying with labelling rules and not exceeding contaminant, residue and microbiological limits. A test result produces evidence not for a certificate but for a functioning system.

Allergen management carries particular weight. The presence of an undeclared allergen in a product is one of the most frequent causes of food recalls. Analysis here runs together with cleaning validation: it is shown that the line has been cleaned adequately after a production run containing an allergen and that the risk of cross-contamination is under control.

Voluntary schemes have become effectively mandatory in this field. Retail chains require their suppliers to hold a certificate under a GFSI-recognised scheme (BRCGS, IFS, FSSC 22000); without it, getting onto the shelf is practically impossible.

Method groups in this field

Pathogen detection
Detection of Salmonella, Listeria monocytogenes, Campylobacter, Cronobacter and Shiga toxin-producing E. coli; culture-based and molecular methods.
Indicator counts
Total mesophilic aerobic count, Enterobacteriaceae, coliforms and E. coli, coagulase-positive staphylococci, yeasts and moulds, lactic acid bacteria, sulphite-reducing Clostridia.
Pesticide and veterinary residues
Multi-residue screening by LC-MS/MS and GC-MS/MS with QuEChERS extraction.
Mycotoxins and contaminants
Aflatoxins, ochratoxin A, deoxynivalenol, patulin; heavy metals (ICP-MS), acrylamide and PAH compounds.
Nutritional composition
Kjeldahl protein, fat and fatty acid profile, moisture, ash, dietary fibre, sugar profile, vitamin and mineral analyses.
Allergens and authenticity
Gluten, milk, egg, nut and soy allergen analyses; molecular methods for species identification and adulteration detection.

Commonly confused in this field

Sampling is half the result. A sample transported at the wrong temperature or delayed gives an invalid result even if it is analysed correctly in the laboratory.
The absence of a pathogen does not show that hygiene is good; indicator counts give separate information and the two are read together.
A result from a sample taken from a lot can be generalised to the whole lot only if the sampling plan was set up statistically.
Limits are defined in separate regulations by product group and are updated regularly; a conformity decision based on an outdated limit table may be wrong.
For exports, the limits of the destination country may differ from EU limits; the same product may be compliant in one market and non-compliant in another.

Which decisions these results support

Verification of the HACCP plan and process monitoring
The basis for the nutrition declaration and allergen information on the label
Health certificates before export and compliance with destination market limits
Supplier and lot-based acceptance control
Shelf-life studies and determining storage conditions
Producing evidence for audits under GFSI-recognised schemes

Related Tests

Frequently Asked Questions About Pesticides

How many active ingredients should be screened?

Determines target market and product. Substances frequently seen in monitoring programs for exports to the EU and risky active substances specific to the product must be on the list. Large screening packages reduce risk but increase cost.

The result is just below the MRL, are we safe?

Measurement uncertainty comes into play. SANTE guidance describes how to take uncertainty into account in the suitability decision. For results close to the limit, additional sample evaluation for the entire batch may be meaningful.

Is it also necessary for organic products?

It is necessary. Organic certification declares that no pesticides have been used, but there may be drift or storage contamination from a neighboring field. Analysis is the verification of the statement.