Foodstuffs - Detection of irradiated foodstuff containing crystalline sugar by ESR spectroscopy

This document specifies a method for the detection of foodstuff containing crystalline sugars which have been treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called electron paramagnetic resonance (EPR) spectrum, of the foodstuff, see [1] to [7].
Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas and raisins, see [1] to [3].

Lebensmittel - ESR-spektroskopischer Nachweis von bestrahlten Lebensmitteln, die kristallinen Zucker enthalten

Dieses Dokument legt ein Verfahren zum Nachweis von mit ionisierender Strahlung behandelten Lebensmitteln, die kristallinen Zucker enthalten, fest. In diesem Verfahren wird das ESR-(Elektronen Spin Resonanz ), auch bekannt als EPR (Elektronen-Paramagnetische-Resonanz)-Spektrum des Lebensmittels analysiert, siehe [1] bis [7].
Ringversuche wurden erfolgreich an getrockneten Feigen, getrockneten Mangos, getrockneten Papayas und Rosinen geprüft, siehe [1] bis [3].

Produits alimentaires - Détection par spectroscopie RPE d’aliments ionisés contenant des sucres cristallisés

Le présent document spécifie une méthode de détection de traitement ionisant appliquée à des aliments contenant des sucres cristallisés, par analyse du spectre de résonance de spin électronique (RSE) aussi appelé spectre de résonance paramagnétique électronique (RPE) des aliments ; voir [1] à [7].
Des essais interlaboratoires ont été réalisés sur des figues, des mangues, des papayes et des raisins déshydratés ; voir [1] à [3].

Živila - Določevanje obsevanosti živil, ki vsebujejo kristalni sladkor, s spektroskopijo ESR

Ta evropski standard določa metodo za določevanje živil, ki vsebujejo kristalni sladkor in so bila obdelana z ionizirajočim sevanjem. Določevanje poteka z analizo elektronske spin resonančne spektroskopije (ESR), imenovane tudi elektronske paramagnetne resonance (EPR), živil.
Medlaboratorijske študije so bile uspešno izvedene na suhih figah, suhih mangih, suhih papajah in rozinah.

General Information

Status
Published
Publication Date
29-Mar-2022
Withdrawal Date
29-Sep-2022
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
30-Mar-2022
Due Date
30-Oct-2021
Completion Date
30-Mar-2022

Relations

Effective Date
06-Apr-2022

Overview

EN 13708:2022 specifies an analytical method using electron spin resonance (ESR, also called EPR) spectroscopy to detect prior ionizing radiation treatment in foodstuffs that contain crystalline sugars. The method is focused on solid, dry parts of food where radiation-induced radicals are stabilized in sugar crystals. Interlaboratory validation has been carried out successfully on dried figs, dried mangoes, dried papayas and raisins.

Key Topics

  • Principle: ESR spectroscopy detects paramagnetic centres (radiation-induced radicals) by measuring microwave absorption under an external magnetic field. Spectra are typically presented as the first derivative of absorption versus magnetic field.
  • Apparatus: Commercial X‑Band ESR spectrometer (magnet, microwave bridge, field controller), ESR tubes (≈4.0 mm internal diameter), balance (1 mg), vacuum oven or freeze dryer and scalpel.
  • Sample preparation: Prepare pieces of fruit (50–100 mg) without grinding; take outer parts where crystalline sugar is more likely. Dry insufficiently dry samples (≈40 °C under reduced pressure or by freeze-drying). Avoid temperatures significantly higher than 40 °C which can reduce the ESR signal.
  • Spectrometer settings (examples): X‑Band frequency ≈9.78 GHz, microwave power ≈5 mW, centre field ≈348 mT, sweep width 10–20 mT, modulation frequency 50–100 kHz, modulation amplitude 0.15–0.4 mT. Settings should be optimized per sample and instrument.
  • Evaluation: Calculate the g‑value from measured frequency and magnetic field to characterise signal centres. Typical identification criteria are provided for certain dried fruits (see Applications).
  • Limitations: Detection requires the presence of crystalline sugar; absence of a multicomponent ESR spectrum does not necessarily prove a sample is unirradiated. Grinding or rehydration can affect signals. Specific radical identification remains limited.

Applications

  • Routine screening of dried fruit imports and foodstuffs for prior irradiation where crystalline sugar is present.
  • Support for food safety, regulatory compliance and inspection activities.
  • Forensic and authenticity testing for producers, laboratories and enforcement bodies.

Practical notes from EN 13708:2022:

  • Dried mangoes and papayas: typical overall spectrum width ≈ 7.4–7.8 mT with a g‑value around 2.0035 ± 0.0010.
  • Dried figs and raisins: typical overall spectrum width ≈ 8.7–9.1 mT with a g‑value around 2.0035 ± 0.0010.
  • Unirradiated samples show either no ESR spectrum or a broad singlet (g ≈ 2.0040 ± 0.0010).

Related Standards

  • EN 1787 (alignment of spectrometer settings and evaluation terminology).
  • Relevant CEN and ISO guidance on sampling, laboratory validation and reporting.

Practical value: EN 13708:2022 provides a validated, portable laboratory approach for identifying irradiation in crystalline‑sugar containing foods. It helps laboratories standardize ESR test procedures, optimize instrument parameters, and report results consistently to support enforcement and trade compliance.

Keywords: EN 13708:2022, ESR spectroscopy, EPR, irradiated food, crystalline sugar, dried fruits, detection method, g‑value, interlaboratory validation.

Frequently Asked Questions

EN 13708:2022 is a standard published by the European Committee for Standardization (CEN). Its full title is "Foodstuffs - Detection of irradiated foodstuff containing crystalline sugar by ESR spectroscopy". This standard covers: This document specifies a method for the detection of foodstuff containing crystalline sugars which have been treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called electron paramagnetic resonance (EPR) spectrum, of the foodstuff, see [1] to [7]. Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas and raisins, see [1] to [3].

This document specifies a method for the detection of foodstuff containing crystalline sugars which have been treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called electron paramagnetic resonance (EPR) spectrum, of the foodstuff, see [1] to [7]. Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas and raisins, see [1] to [3].

EN 13708:2022 is classified under the following ICS (International Classification for Standards) categories: 67.050 - General methods of tests and analysis for food products. The ICS classification helps identify the subject area and facilitates finding related standards.

EN 13708:2022 has the following relationships with other standards: It is inter standard links to EN 13708:2001. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

EN 13708:2022 is associated with the following European legislation: EU Directives/Regulations: 2017/625, 882/2004. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

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Standards Content (Sample)


SLOVENSKI STANDARD
01-junij-2022
Nadomešča:
SIST EN 13708:2002
Živila - Določevanje obsevanosti živil, ki vsebujejo kristalni sladkor, s
spektroskopijo ESR
Foodstuffs - Detection of irradiated foodstuff containing crystalline sugar by ESR
spectroscopy
Lebensmittel - ESR-spektroskopischer Nachweis von bestrahlten Lebensmitteln, die
kristallinen Zucker enthalten
Produits alimentaires - Détection par spectroscopie RPE d’aliments ionisés contenant
des sucres cristallisés
Ta slovenski standard je istoveten z: EN 13708:2022
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 13708
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2022
EUROPÄISCHE NORM
ICS 67.050 Supersedes EN 13708:2001
English Version
Foodstuffs - Detection of irradiated foodstuff containing
crystalline sugar by ESR spectroscopy
Produits alimentaires - Détection par spectroscopie Lebensmittel - ESR-spektroskopischer Nachweis von
RPE d'aliments ionisés contenant des sucres bestrahlten Lebensmitteln, die kristallinen Zucker
cristallisés enthalten
This European Standard was approved by CEN on 14 February 2022.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13708:2022 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Apparatus and equipment . 5
6 Procedure. 5
7 Evaluation . 6
8 Limitations . 8
9 Validation . 8
10 Test report . 9
Annex A (informative) Example Figures . 10
Bibliography . 12
European foreword
This document (EN 13708:2022) has been prepared by Technical Committee CEN/TC 275 “Food
analysis - Horizontal methods”, the secretariat of which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by September 2022, and conflicting national standards shall
be withdrawn at the latest by September 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 13708:2001.
The predecessor of this document was elaborated on the basis of a protocol developed following a
concerted action supported by the Commission of European Union (XII C.). Experts and laboratories from
E.U. and EFTA countries, contributed jointly to the development of this protocol.
In comparison with the previous edition, the entire document was editorially revised according to
current rules. Additionally, the following technical modifications have been made:
a) clause “Normative references” was added;
b) clause “Terms and Definitions” was added;
c) former 3.2 was scientifically refined and converted into a footnote;
d) section “Sample preparation” was slightly extended and modified by conversion of the NOTE and
WARNING into main text;
e) section “Spectrometer settings” was scientifically refined, its normative character (i.e. provisions set
out) modified towards more exemplary/suggestive expressions of provision and aligned with
EN 1787;
f) clause “Evaluation” was amended by restructuring the subsections (subsection “G-value calculation”
became 7.1 and “Identification of irradiated samples” 7.2), including refinement of the given
information, designations and abbreviations including the alignment with the Annexes and EN 1787;
g) clause “Limitations” was extended;
h) layout of Figures A.1 to A.4 were revised and Figures A.5 to A.7 for irradiated fructose, glucose and
saccharose were added including alignment of the given information with the main text and EN 1787;
i) the Bibliography was updated and extended by entry [8], [9] and [10].
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
1 Scope
This document specifies a method for the detection of foodstuff containing crystalline sugars which have
been treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called
electron paramagnetic resonance (EPR) spectrum, of the foodstuff, see [1] to [7].
Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas
and raisins, see [1] to [3].
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
ESR spectroscopy detects paramagnetic centres (e.g. radicals). They are either due to irradiation or to
other compounds present. An intense external magnetic field produces a difference between the energy
levels of the electron spins m = +½ and m = -½, leading to resonance absorption of an applied
s s
microwave beam in the spectrometer. ESR spectra are conventionally displayed as the first derivative of
the absorption with respect to the applied magnetic field.
The magnetic field and microwave frequency values depend on the experimental arrangements (sample
size and sample holder), while their ratio (i.e. g value) is an intrinsic characteristic of the paramagnetic
centre and its local co-ordination. For further information, see [1] to [7].
Radiation treatment produces radicals, which can be mostly detected in solid and dry parts of the
foodstuff. The intensity of the signal obtained increases with the concentration of the paramagnetic
compounds and thus with the applied dose.
5 Apparatus and equipment
Usual laboratory apparatus and, in particular, the following.
5.1 Commercially available X-Band ESR spectrometer including magnet, microwave bridge, console
with field-controller and signal-channel, rectangular or cylindrical cavity .
®2
5.2 ESR tubes, with an internal diameter of about 4,0 mm (e.g. Suprasil quartz tubes).
5.3 Balance, accuracy of 1 mg (optional).
5.4 Laboratory vacuum oven, or freeze dryer.
5.5 Scalpel.
6 Procedure
6.1 Sample preparation
Prepare suitable pieces (50 mg to 100 mg) of the fruits, e.g. using a scalpel. Avoid grinding of samples.
Various parts of the fruits can contain different quantities of crystalline sugars. It can be advantageous to
take the test sample from the outer parts of the fruits.
Transfer a test portion directly into the ESR tube (5.2) and start the measurement.
Difficulties in tuning the spectrometer cavity can be experienced if the sample is insufficiently dry. In this
case either reduce the sample quantity or dry it further. Samples should be dried in a laboratory vacuum
oven at approximately 40 °C under reduced pressure or in a freeze-dryer.
Temperatures significantly higher than 40 °C can reduce the signal.
6.2 ESR Spectroscopy
6.2.1 Spectrometer settings
The parameters shown in Table 1 have been found to be successful in interlaboratory tests (see Clause 9).
The values shown (Table 1) are gi
...

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표준 EN 13708:2022는 방사선 조사된 결정형 설탕을 포함한 식품의 검출을 위한 ESR 분광법(전자 스핀 공명 스펙트럼)을 규정하는 문서로, 이 표준의 주요 범위와 강점은 다음과 같습니다. 이 표준은 이온화 방사선으로 처리된 결정형 설탕이 포함된 식품의 식별을 위한 방법론을 명시하며, 이를 통해 식품의 안전성을 확보하고 품질을 유지하는 데 중요한 역할을 합니다. 특히, 전자 스핀 공명(EPR) 스펙트럼 분석을 통해 식품이 방사선 조사되었는지를 정확하게 판단할 수 있습니다. 또한, 표준의 강점으로는 다양한 식품에 대한 실험실 간 연구가 성공적으로 수행되었다는 점을 들 수 있습니다. 말린 무화과, 말린 망고, 말린 파파야 및 건포도와 같은 다양한 샘플을 대상으로 한 연구 결과는 신뢰성이 높으며, 이러한 연구들은 이 표준의 적용 가능성과 신뢰성을 더욱 강화합니다. EN 13708:2022는 방사선 처리 식품의 검출이라는 특정하고도 중요한 문제를 해결하는 데 있어서 필수적인 문서이며, 식품 안전 및 소비자 보호의 관점에서 큰 의미를 갖습니다. 이 표준은 앞으로도 식품 산업에서 방사선 조사식품의 관리와 감시에 중요한 역할을 지속할 것으로 기대됩니다.

Die Norm EN 13708:2022 legt einen klaren und präzisen Rahmen für die Detektion von Lebensmitteln, die Kristallzucker enthalten und ionisierender Strahlung ausgesetzt wurden, fest. Die Anwendung der Elektronenspinresonanz (ESR) Spektroskopie zur Analyse von Lebensmitteln stellt einen innovativen Ansatz dar, der wertvolle Informationen über die Strahlenbehandlung liefert. Ein bedeutender Stärke dieser Norm liegt in ihrer Methodik. Die Verwendung der ESR-Spektroskopie, auch als Elektronenspinspektroskopie bekannt, ermöglicht eine hochgenaue Identifizierung der behandelten Lebensmittel. Durch die detaillierte Analyse des ESR-Spektrums können Rückschlüsse auf die Qualität und Sicherheit der Lebensmittel gezogen werden, was besonders in einer Zeit von wachsendem Verbraucherbewusstsein über Lebensmittelverarbeitung von hoher Relevanz ist. Darüber hinaus wurden erfolgreiche Interlaboratorienstudien an einer Reihe von getrockneten Früchten – einschließlich getrockneter Feigen, Mango, Papaya und Rosinen – durchgeführt. Diese umfassenden Tests belegen die praktische Anwendbarkeit der Norm und stärken deren Vertrauenswürdigkeit in der Lebensmittelanalyse. Insgesamt bietet die EN 13708:2022 eine unverzichtbare Grundlage für die Detektion von bestrahlten Lebensmitteln mit Kristallzucker. Durch ihre sorgfältige methodische Herangehensweise, die geprüfte Effektivität in internen Studien und die breite Relevanz für Lebensmittelsicherheit ist diese Norm ein essentielles Werkzeug für die Lebensmittelindustrie und Verbraucher.

EN 13708:2022の標準は、結晶性糖を含む食品の放射線照射の検出方法に関して詳細に規定されており、食品業界における重要な文書となっています。この標準は、電子スピン共鳴(ESR)スペクトル、または電子パラマグネット共鳴(EPR)スペクトルを用いて、イオン化放射線で処理された食品を分析する手法を明確にしています。 この標準の強みは、干しイチジク、干しマンゴー、干しパパイヤ、レーズンといった具体的な食品を対象にしたインタラボラトリースタディの成功に裏打ちされている点です。これにより、検出方法の実用性と信頼性が高められており、食品の品質管理や安全性評価に貢献しています。さらに、結晶性糖を含む食品に特化することで、特定のニーズに応じた検査方法を提供し、業界内での適用範囲を広げています。 この標準は、食品の放射線照射に関する国際的な基準を満たすための基盤を提供するものであり、食品安全に対する意識が高まる中で、その重要性はますます高まっています。従って、EN 13708:2022は、食品産業における信頼性の高い検出手法を確立し、この分野での研究および開発の進展に寄与するものと言えます。

The EN 13708:2022 standard provides a comprehensive framework for the detection of irradiated foodstuffs containing crystalline sugars through the utilization of electron spin resonance (ESR) spectroscopy. The scope of this standard is crucial in addressing the growing concerns related to food safety and consumer health, particularly in the context of food irradiation practices. One of the strengths of the standard lies in its scientific approach to analyzing the ESR spectrum, enabling precise identification of foods treated with ionizing radiation. This method is particularly relevant as it expands our understanding and capability to monitor food quality, ensuring that consumers are informed about the safety and treatment of the food products they consume. The inclusion of interlaboratory studies conducted on various dried fruits, such as figs, mangoes, papayas, and raisins, demonstrates the robustness and applicability of the method across different food matrices. This empirical foundation enhances the credibility of the standard and builds trust in its results. Furthermore, EN 13708:2022 aligns with international food safety regulations, making it a pivotal reference for manufacturers, regulators, and testing laboratories concerned with food irradiation. By standardizing the detection methods, it aids in achieving consistency and reliability across different testing environments, which is essential in maintaining the integrity of food safety measures. In summary, the EN 13708:2022 standard stands out for its methodological rigor and relevance in contemporary food safety practices, providing essential guidance for the detection of irradiated foods containing crystalline sugars. Its strengths in empirical validation through interlaboratory studies and compatibility with international standards reinforce its importance in the food industry.

Le document SIST EN 13708:2022 constitue une avancée significative dans le domaine de la détection des denrées alimentaires irradiées, en mettant l'accent sur les aliments contenant des sucres cristallins. Ce standard définit une méthode précise pour l'identification des aliments ayant subi un traitement par rayonnement ionisant, à travers l'analyse du spectre de résonance de spin électronique (ESR), également connu sous le nom de résonance paramagnétique électronique (EPR). L'un des principaux points forts de cette norme est sa capacité à fournir une méthode fiable et scientifique pour déterminer la présence de traitements par radiation dans les aliments, ce qui est crucial pour assurer la sécurité alimentaire et la transparence dans la chaîne d'approvisionnement. Les études interlaboratoires menées avec succès sur des échantillons tels que les figues séchées, les mangues séchées, les papayes séchées et les raisins renforcent la crédibilité du standard, attestant de sa capacité à être appliqué sur une variété de produits. En outre, le document soutient la lutte contre la fraude alimentaire, en garantissant que les produits exposés aux rayonnements ionisants sont correctement identifiés et que les consommateurs sont informés. La pertinence de cette norme est indéniable dans un contexte où la traçabilité et la sécurité des aliments sont devenues des priorités majeures pour les régulateurs et les consommateurs. En résumé, le SIST EN 13708:2022 joue un rôle essentiel dans le domaine de l'analyse des denrées alimentaires, offrant une méthodologie robuste pour la détection des aliments traités par ionisation, et contribuant ainsi à une chaîne alimentaire plus sécurisée et transparente.