方案详情文
智能文字提取功能测试中
JRC TECHNICAL REPORTS Guidance on sampling, analysis and datareporting for the monitoring of mineral oilhydrocarbons in food and food contactmaterials In the frame of CommissionRecommendation (EU)2017/84 S. Bratinova, E. Hoekstra (Editors) 2019 This publication is a Technical report by the Joint Research Centre (JRC), the European Commission’s science and knowledge service. It aimsto provide evidence-based scientific support to the European policymaking process. The scientific output expressed does not imply a policyposition of the European Commission. Neither the European Commission nor any person acting on behalf of the Commission is responsiblefor the use that might be made of this publication. Contact informationStefanka BratinovaEuropean Commission, Joint Research Centre (JRC)European Union Reference Laboratory for Food Contact MaterialsVia Enrico Fermi, 2749, TP260, 21027 Ispra (VA), Italy JRC-FCM@ec.europa.eu JRC Science Hub https://ec.europa.eu/jrc JRC115694 EUR 29666 EN PDF ISBN 978-92-76-00172-0 ISSN 1831-9424 doi:10.2760/208879 Luxembourg: Publications Office of the European Union, 2019 C European Union, 2019 Reuse is authorised provided the source is acknowledged. The reuse policy of European Commission documents is regulated byDecision 2011/833/EU (OJ L 330,14.12.2011, p.39). For any use or reproduction of photos or other material that is not under the EU copyright, permission must be sought directly from thecopyright holders. How to cite this report: S. Bratinova, E. Hoekstra (Editors) Guidance on sampling, analysis and data reporting for the monitoring of mineraloil hydrocarbons in food and food contact materials, Luxembourg: Publications Office of the European Union, 2019 ISBN 978-92-76-00172-0, doi:10.2760/208879, JRC115694 All images C European Union 2019 Contents Acknowledgements..... ..2 Executive summary....... ..3 1Introduction ...... ..4 2SScope.......... ..5 3. Sampling....... ..6 4Analysis....... .10 4.1Description of the mineral oil hydrocarbons.... .10 4.2 Definition of the measurands........ .11 4.3Background of MOH analysis......... . .m .11 4.4Outline of the analytical approach.. .12 4.5 Verification of the method performance....... .14 4.6 Quantification...... .15 4.77IPerformance requirements of the analytical methods....... .16 5Reporting of results.......... .19......................m ...............................................i................................... .List of abbreviations ....... .27 Annexl...... .28 Annexll......31 Acknowledgements This Guidance has been prepared by the Task Force on Mineral Oil established by the EuropeanUnion Reference Laboratory for Food Contact Materials (EURL-FCM). Members of the Task Force are experts from National Reference Laboratories (NRL) for Food ContactMaterials, experts of food analysis and representatives from DG SANTE and the EURL-FCM: Maurus Biederman and Gregor McCombie (Kantonales Labor Zurich,NRL-CH) Dimitrios Chrysafidis (General Chemical State Laboratory of Greece, EL) Isabelle Deyris and Ronan Jaouannet (Service commun des laboratoires DGDDI et DGCCRF,NRL-FR) Liam Dolan (Health Service Executive,NRL-IE) Thomas Funke and Christophe Goldbeck (Chemisches und VeterinaruntersuchungsamtMunsterland-Emscher-Lippe, DE) Carmen Igualda and Yovana Sanchis (La Fundacion para el Fomento de la InvestigacionSanitaria y Biomedica de la Comunitat Valenciana (Fisabio), ES) Jurg Daniel (Amt fur Verbraucherschutz und Veterinarwesen AVSV St. Gallen, CH) ● Oliver Kappenstein (Bundesinstitut fur Risikobewertung, NRL-DE) Verena Koospal (Chemisches und Veterinaruntersuchungsamt Stuttgart, DE) Wenceslao Moreda (Instituto de la Grasa (IG), Centro de Investigacion de la Agencia EstatalConsejo Superior de Investigaciones Cientificas (CSIC), ES) Els van Hoeck (Scientific Institute of Public Health (WIV-ISP), NRL-BE) Bastiaan Schupp, Veerle Vanheusden and Frans Verstraete (European Commission, DGSANTE) Stefanka Bratinova, Eddo Hoekstra, Giorgia Beldi, Natalia Jakubowska, Lubomir Karasek, PiotrRobouch, Sandro Valzacchi (EURL-FCM,European Commission, Joint Research Centre (JRC)) Furthermore, the following EFSA colleagues are acknowledged for their input to the reporting sectionof this guidance: Marco Binaglia, Stefano Cappe, Valentina Bocca, Davide Gibin, Monica Giulivo andGiulio Di Piazza. Executive summary This guidance document covers specific directions for sampling and analysis of mineral oil saturatedhydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in food and FCM in the frameof Recommendation (EU) 2017/84 for the monitoring of mineral oils. It provides guidance on the minimum performance requirements of the analytical methods fit forMOSH/MOAH monitoring. The guidance should be used by all stakeholders involved in thedetermination of mineral oil hydrocarbons in food and FCM, i.e. food inspectors, official controllaboratories, laboratories in industry and laboratories of non-governmental organisations. This guidance aims to support the generation of reliable data for the occurrence of both fractions -MOSH and MOAH- and to enable reporting by laboratories that are already familiar with theanalytical approaches and have proven their analytical performance in relevant proficiency testing(PT) schemes. For laboratories that are not familiar with MOSH/MOAH analysis, this guidance gives the minimumperformance requirements and references to current analytical approaches described in thescientific literature. It does not provide standard operating procedures. 1.Introduction consumers are exposed to a range of mineral oil hydrocarbons (MOH) via food. Major sources ofMOH in food are food packaging and additives, processing aids, and lubricants. Technical grade MOHcontains up to about 50 % mineral oil aromatic hydrocarbons (MOAH); approved food grade mineraloil saturated hydrocarbons (MOSH) (white oils) are reported to contain less than 1 % of MOAH.Estimated MOSH exposure ranges from 0.03 to 0.3 mg/kg b.w. per day, with higher exposure inchildren. Except for white oils, exposure to MOAH is about 20 % of that of MOSH. In 2012, the Scientific Panel on Contaminants in the Food Chain (CONTAM Panel) of the EuropeanFood Safety Authority (EFSA), on request by the Commission, issued an Opinion' concluding that thepotential human health impact of groups of substances among the MOH vary widely. Occurrence data were available only for a limited number of food groups and only from a fewcountries. At that time MOAH measurements did not exist for the majority of the samples. Until2009, only the MOSH fraction was routinely analysed. Then it was possible to extend the method tothe MOAH fraction. MOAH, however, may act as genotoxic carcinogens, while some mineral oilsaturated hydrocarbons (MOSH) can accumulate in human tissue and may cause adverse effects inthe liver. As some MOAH are considered mutagenic and carcinogenic, it is important to organisemonitoring of MOH to better understand the relative presence of MOSH and MOAH in foodcommodities that are major contributors to dietary exposure. Commission Recommendation (EU) 2017/84 requests the Member States to monitor animal fat,bread and rolls (including fine bakery ware), breakfast cereals, confectionery (including chocolateand cocoa), fish meat, fish products (canned fish), grains for human consumption, ices and desserts,oilseeds, pasta, sausages, tree nuts, vegetable oil. It is required to sample food and pre-packagedfood and to analyse the food and, if relevant, food contact materials (FCM) as well for the presenceof mineral oil and to report the results to EFSA. The analysis of MOH in food and FCM, especially in food with high fat content, is very demanding interms of methodology and interpretation. It requires harmonisation amongst laboratories in terms ofdefinitions, performance characteristics and data reporting to EFSA. According to the Recommendation (EU) 2017/84 "to ensure the reliability of the obtained analyticaldata, Member States should ensure the availability of suitable analytical equipment and gainsufficient experience in the analysis of MOH both in food and in FCM before generating analyticalresults. To ensure the uniform application of this recommendation, the European Union ReferenceLaboratory for FCM (EU-RL) should provide further guidance to the competent authorities of theMember States and other interested parties, including guidance on information that could becollected during investigations, as well as methods of sampling and analysis ... the Member Statesshould collaborate with the EU-RL to jointly develop that guidance in accordance with their needs fordeveloping analytical capabilities." Following the Recommendation, this guidance document aims at giving directions to the MemberStates with respect to sampling, describing the performance characteristics of the analyticalapproaches,as well as defining the way the results should be reported to EFSA. ( E FSA (2012) Scientific Opinion on Mineral Oil Hydrocarbons in Food. EFSA Journal 1 0 (6), 2704. ) ( 2 B iedermann M, Fiselier K, Grob K. (2009)J Agric Food Chem 57, 8711. ) 2Scope This guidance document has been developed for supporting the implementation of CommissionRecommendation (EU) 2017/84. It provides guidance on sampling, analysis and reporting of theresults for the content of total MOSH and MOAH and various carbon fractions of MOSH and MOAH.This guidance shall be used by food inspectors, official control laboratories, commercial laboratories(independent and industry) and laboratories of non-governmental organisations that monitormineral oil in food and FCM. This guidance aims to 1facilitate harmonised sampling of food and FCM for MOSH and MOAH analysis;2 facilitate harmonised reporting to EFSA by laboratories that are already familiar with theanalytical approaches and have proven their analytical performance in relevant proficiencytesting (PT) schemes; 3. give the essential performance requirements for the methods to be applied in MOSH/MOAHanalysis; 4. give references to current analytical approaches described in the scientific literature forlaboratories that are not familiar with the analytical methodology This guidance does not aim to provide standard operating procedures. If other guidance or standard operating procedures are necessary, these would be developed in theframe of future planned hands-on training courses. This guidance should enable stakeholders to sample, analyse and report mineral oils in food and, ifrelevant, in FCM in a harmonised manner. 33Sampling Recommendation (EU) 2017/84 refers explicitly to Regulation (EC) No 333/2007 laying down themethods of sampling and analysis for sampling food, and relating to the control of lead, cadmium,mercury, inorganic tin, inorganic arsenic, 3-MCPD and polycyclic aromatic hydrocarbons in food. Only the following sections of this Regulation are relevant for sampling procedures for mineral oil infood: Annex Part A; Annex Part B: sections B.1.1 (just for official control); B.1.2 to B.1.6, B.1.7 (firstparagraph); B.1.8; B.2 (not the last paragraph related to tin B.2.2); and B.3. Since Recommendation (EU) 2017/84 does not concern official controls, strict adherence toRegulation (EC) No 333/2007 is not obligatory in the context of mineral oil monitoring. In the following paragraph the guidance applies to sampling, where the main focus is on collectingfrom different suppliers as many products as possible in a given food category as listed inRecommendation (EU) 2017/84. Guidance for sampling As the focus of the Guideline is on monitoring and not official control, it is not obligatory to followsections B.1.2, B.1.4 and B.1.5 for the sampling of mineral oil in lots and sub-lots. Moreover, it is not obligatory to adopt section B.1.6, particularly in taking samples for enforcement,defence and referee purposes. If unused packaging material from the same batch that was used to package the food is still availableat the food business operator, then it should also be sampled as it may provide useful information toidentify the source of any contamination that is found in the packaged food. The person performing sampling should take all necessary precautions to avoid contamination of thesample. For example, the use of cosmetics such as hand creams should be avoided. The sample collection tools should be free from mineral oil contamination. Unpackaged food should be sampled in containers which are inert for mineral oil. Only containersthat are impermeable to MOH, do not release interfering substances and do not adsorb MOH, shouldbe used. Glass or polyethylene terephthalate (PET) containers have the identified properties and aremostpreferred. Each new batch of sample containers should be checked for mineral oilcontamination. If a mineral oil contamination is detected, the containers should be washed beforeuse with purified n-hexane and dried at the highest temperature possible. Glass sample containerscould also be annealed, preferably at 400 ℃. Mineral oil contamination of sample containers needsto be checked for each new batch after such treatment. NOTES: Polyolefin sample containers, made of, e.g. polyethylene or polypropylene, may release polyolefinoligomeric hydrocarbons (POH). These containers are not suitable unless appropriate precautionssuch as lining with aluminium foil are taken to prevent contamination of the samples. Metal sample containers and aluminium foil may have a mineral oil film on their surface due totheir production. These containers would only be suitable upon ensuring that they are free ofmineral oil residues. The mineral oil residues could be removed by rinsing with purified n-hexane. Paperboard boxes are generally not suitable even for the secondary packaging of the samples. After collecting the sample, the sample container should be closed with a Polytetrafluoroethylene(PTFE)-layered lid or a glass stopper. Otherwise, the sample container must be covered first withaluminium foil before being sealed with its cap or stopper. The aluminium foil also needs to be checked for residual mineral oil contamination on its surface. No rubber rings should be used to closethe container. Pre-packaged food or FCM should be wrapped in aluminium foil at the point of sampling and keptwrapped until being analysed to prevent cross-contamination. If the pre-packaged food sample isbrought into the laboratory without being wrapped in aluminium foil,this should be documented. All contamination of the sample, e.g. by the use of tape or adhesives (paper/plastic labels) or contactwith paper or paperboard, should be prevented. However, the sample must remain properlyidentifiable, e.g. by using a permanent marker. If glass sample containers cleaned in a washing machine are reused, then the efficiency of thewashing procedure should be checked. Reused sample containers do not need to be checked forresidual mineral oil contamination if the washing procedure was effective in removing such residues. No tape or adhesives (paper/plastic labels) should be used to fix the aluminium foil that covers thepre-packaged food. The sample identification number should be written on the aluminium foil using a permanentmarker. Recording of information during sampling The following information on the food sample should be recorded. The relevant EFSA reporting dataelements are mentioned in brackets. EFSA requirements 3laid down in the Standard Sample Description on Food and Feed (SSD1) are: Laboratory sample code (S.01) - expressed by a unique sample identification number, not longerthan 20 characters. Country of sampling (S.04) - This is the country where the food was selected for laboratorytesting. Country of origin of the product (S.06)- This is the country where the food originated. Area of origin for fisheries or aquaculture activities code (S.08)- FAO Fisheries areas. EFSA Product code (S.12)- Food products should be described according to the FoodExcatalogue of the Standard Sample Description (SSD). It is mandatory to report, at least, level 2 ofthe FoodEx code. It is strongly encouraged to classify the food samples at the most detailedhierarchical level available (FoodEx level 3 and 4). This is particularly needed for food groups like"Food for infants and small children” and “Products for special nutritional use”, where anyavailable additional descriptions shall be provided. Specific attention needs to be given to the reporting of data on cereal grains. It is essential tomake a clear distinction between grains as harvested (unprocessed grains of undefined use, notfor human exposure assessment), grains for human consumption, and grains as feed. Product full-text description (S.14) - This is essential to check if the EFSA product code (FoodExcode) given by the data provider is consistent with the text description. This will avoid anypossible mistakes in coding and additional clarification requests. Also, as this is a free textelement, the information could be provided even in the national language. The originaldescription of the sample from the national database can be copied here. It should be avoidedto repeat just the FoodEx description. Moreover, any additional information that does notbelong to any of the other SSD fields should be reported in S.14. ( EFSA (2010) Standard sa m ple description for food an d feed. EF S A Journal 8(1), 1457 ) ● Packaging (S.16)- Describe the container or wrapper that holds the product, e.g. multi-layermaterial or inner bag incl., further information on the material of layers; the presence of abarrier and assembled packaging material. Product treatment (S.17) - It is mandatory to indicate explicitly if the original sample is treatedor not, especially if it is a dehydrated product. Product comment (S.21)-Additional information on the product, particularly preparation detailsif available. Year, month and day of expiry (S.25, S.26, S.27) - Best-before date or use by year or otherindications of the expiry date. ● Year, month and day of sampling (S.28, S.29, S.30)- If the sample is the result of sampling over agiven period, this field should contain the year, month or day when the first sample wascollected. Sampling strategy (S.33)- It is mandatory to describe how the sample was selected from thepopulation being monitored or surveyed. . Programme type (S.34)-The sampling programme type must be reported to indicate the type ofcontrol programme or other types of the source to which the sample belongs. Sampling method (S.35)- It is mandatory to define the way the samples were collected foranalysis. In the case of aggregated samples, the number of the incremental samples should bereported. Sampling point (S.39)- Point in the food chain where the sample was taken. History of the food or pre-packaged sample- e.g. about possible contamination sources duringfood processing or contact with secondary packaging, transport boxes, jute bags, batching oils"(R.32). Additional information: Article number. European Article Numbering (EAN) code . Batch or lot number. ● Total mass of aggregated food sample. ● Labels (physically or photocopy)- In the context of pre-packaged food in paper and board, themass of the food and the packaging needs to be determined. Mass of packaged food sample (if possible). Mass of packaging material (if possible). Table I summarises the minimum number of incremental samples to be taken and the mass of theincremental samples depending on the mass of the (sub) lot of the non-packaged products. ( T oolbox for Preventing t he T ransfer of Undesired M ineral Oil H ydrocarbons i n to Food (2017) G e rman Fed e ration of Food Law and Food Science (B l l e. V ). ht t p s: //www.bll.de/download/to o lb o x-for-preven t ing-t h e - transfer-of-undesired-mineral - oi l -hydrocarbons- into-food 5 ) ( https://en.wikipedia.org/wiki/International Ar t icle Number ) Tablel Minimum number of incremental samples to be taken and the mass or volume of theincremental samples depending on the mass of the lot of the non-packaged products product type lot mass(ton) no. sublot (sub)lot mass (kg) min. no. of incremental samples min. amount of incremental sample (g or ml) bulk products ≥100 ≥1 >500 10 100 <100 1 >500 10 100 <100 1 ≥50 and≤500 5 200 <100 1 <50 3 330 other products ≥15 ≥1 > 500 10 100 <15 1 >500 10 100 <15 1 ≥50 and ≤ 500 5 200 <15 1 <50 3 330 bulk homogeneousliquid products ≥1 3 330 4 Analysis 4.1L Description of the mineral oil hydrocarbons Mineral oil hydrocarbons (MOH) are a complex mixture of hydrocarbons, which originate from crudemineral oils or which are produced from coal, natural gas or biomass through Fischer-Tropschsynthesis. MOH does not include hydrocarbons: - naturally occurring in food: such as n-alkanes of odd numbered carbons (from C21 to C35) ornatural olefins of terpenic origin (such as squalene, sterene or carotenoids ). - such as POH (polyolefin oligomeric hydrocarbons) potentially migrating from plastic packaging(e.g. polyethylene or polypropylene packaging) or synthetic isoparaffins with short and long sidechains used e.g. in synthetic lubricants and adhesives. MOH are divided into two main types-MOSH and MOAH. Mineral oil saturated hydrocarbons (MOSH)° MOSH comprise paraffins (open chain hydrocarbons) and naphthenes (cyclic hydrocarbons), whichare mostly highly alkylated and originate either directly from mineral oil or are formed duringrefining by hydrogenation of aromatic compounds or other conversion processes. Paraffins (open chain hydrocarbons) are distinguished from naphthenes (hydrocarbons with at leastone saturated ring). Paraffins can be grouped into the linear n-alkanes (those with at least about 20carbons are forming waxes) and the branched hydrocarbons, usually being liquids. Naphthenes tendto be highly alkylated and originate either from mineral oil or from hydrogenation of aromatics. Mineral oil aromatic hydrocarbons (MOAH)° MOAH contain at least one aromatic ring. They include polyaromatic compounds, but should bedistinguished from the compounds commonly termed polyaromatic hydrocarbons (PAH), such asbenzopyrenes, which are formed at high temperatures. PAH are only slightly alkylated and can beanalysed as individual substances, whereas MOAH are usually alkylated to more than 98 %, consistof large numbers of compounds and form broad chromatographic signals (humps) with hardly anysharp peak signal on top. Polyolefin oligomeric hydrocarbons (POH) POH are oligomers of polyolefins, such as polyethylene, polypropylene and polybutylenes. FCM usescomprise plastic bags, containers or films, sealable heat layers (e.g. in aluminium bags) and otherlamination as well as adhesives and plasticisers. The POH that are potentially relevant for humanhealth and determined by the described method are at the low end of the molecular mass range ofthe oligomers. They largely consist of branched hydrocarbons, sometimes mono-unsaturatedhydrocarbons and are eluted from the HPLC column in the MOSH fraction. POH may sometimes bedistinguishable from MOSH by their chromatographic pattern, but it is difficult (and for some POHimpossible) to differentiate and chromatographically separate them from the MOSH if both arepresent. Poly Alpha Olefins (PAO)° Similar to POH, PAO are isoparaffins with short main hydrocarbon chains and long side chains ofsynthetic origin.Usually they can be identified by their characteristic chromatographic pattern. ( Biedermann M., Grob K. (2012). Journal of Chrom. A 1255,56 ) ( ' G rob K ., B iedermann M., Caramaschi A., P acciarelli B. (1 9 91) J. High Resolut. Ch r omatogr. 14, 33 ) ( °Biedermann M., GrobK. (2012) Journal of Chrom. A 1255, 76 ) 4.2 Definition of the measurands For the analytical determination of the MOSH/MOAH content in food and FCM measurands have tobe defined, which reflect the MOSH/MOAH descriptions above. MOSH The total MOSH measurand is defined as the total mass fraction of MOSH - expressed inmg MOSH / kg sample -after separation from MOAH and removal of all possible interferences in theextract, as quantified by integration of the whole signal interval in the GC/FID chromatogrambetween the retention times of the peak start of n-C10 and the peak end of n-Cso after subtracting theidentified sharp peaks not belonging to MOSH and using cyclohexylcyclohexane (CyCy) as internalstandard (IS). Another hydrocarbon could be used as IS, provided its response factor is identical. Other detectiontechniques are acceptable, provided that equivalent results are demonstrated. The MOSH fraction may include polyolefin oligomeric hydrocarbons and hydrocarbons from polyalpha olefins (PAOs) in case where their separation/substraction is impossible. The presence of POHand/or POA should be clearly reported. MOAH The total MOAH measurand is defined as the total mass fraction of MOAH - expressed inmg MOAH/ kg sample - after separation from MOSH and removal of all possible interferences in theextract, as quantified by integration of the whole signal interval in the GC/FID chromatogrambetween the retention times of the peak start of n-Ci0 and the peak end of n-Cso after subtracting theidentified sharp peaks not belonging to MOAH and using 1-or 2-methylnaphthalene as IS. Another hydrocarbon could be used as IS, provided its response factor is identical. Other detectiontechniques are acceptable, provided that equivalent results are demonstrated. 4.3 Background of MOH analysis Over the past decade several approaches have been suggested for the determination of MOSH andMOAH in FCM and food, all of them having certain advantages and drawbacks. MOSH/MOAHseparation and its subsequent determination could be achieved by applying on-line LC-GC-FID, off-line HPLC followed by GC-FID or manual off-line separation of MOSH/MOAH followed by GC-FID. It is not possible to separate the mineral oils into single components because they typically contain acomplex mixture of alkanes and other compounds. The combination of LC, which separates MOSHfrom MOAH, and GC-FID for quantification allows for an appropriate determination of the MOSH andMOAH content. In the GC-FID chromatograms of the MOSH and MOAH fractions, further fractionscan be defined based on the retention time of the corresponding n-alkanes under the samechromatographic conditions. It has been decided in agreement with EFSA to collect data for mineraloils up to n-Cso atoms in their molecules in order to reflect the composition of some lubricant oil withheavier oil fractions. Until recently, all the reported data included only hydrocarbons up to n-C40. On-line LC-GC has the advantages of high separation efficiency, high sample throughput, reducedsolvent consumption and sample manipulation, thus enhancing the reproducibility of the method.On-line LC-GC-FID analysis enables the re-use of the same LC column. Solvent consumption is lowerthan with most conventional liquid chromatographic sample preparation methods, including solid ( Biedermann-Brem, Kas p rick N., Simat T., G r ob K. ( 2 012) Food Addit.Contam. A 29, 449. ) phase extraction (SPE). On-line coupling to GC is integrating sample preparation into the final analysisand is fully automating rather complex procedures. As it is a closed system, it also avoidscontamination during sample preparation, which is of particular importance for analytes that arewidely present in laboratories, such as mineral oil hydrocarbons. On the other hand, the sensitivity islimited by the capacity of the LC column. Dedicated instrumentation and skilled operators arerequired. An LC column could also be applied for a pre-separation in the off-line mode by collecting the MOSHand MOAH fractions using automated fraction collectors. LC separating columns with a largerinternal diameter (4.6 mm instead of 2 mm) could be used for this approach. A larger sample couldbe injected into the LC column compared to on-line coupling. In order to achieve similar detectionlimits as in on-line coupling, a fifth of the fraction should be injected into the GC. Nevertheless itrequires larger volume injection in the GC system even if the fractions are significantly enrichedbeforehand. This is the greatest challenge of this technique, in addition to contamination-relatedproblems that could occur during the collection of the MOSH and MOAH fractions. The third possibility is to follow a pure "off-line" method, using a glass column filled with silica/AgNOgto separate the MOSH and MOAH fractions1. The method is very time consuming and requires strictmeasures to prevent contamination of the sample from the consumables and the environment. Flame ionisation detection (FID) is neither sensitive nor selective. It provides almost identicalresponses to all hydrocarbons, making it a preferred detector for MOSH/MOAH quantifications.However, due to the lack of selectivity, additional sample preparation techniques to eliminateinterferences and to enrich both MOSH and MOAH’fractions may need to be applied. Until now, most of the data on the MOSH and MOAH content in foods and FCM were produced afterapplying chromatographic separation using automated on-line coupled LC-GC and quantification byFID. Today, the LC-GC-FID method is referred to as the method of choice for the quantification of mineraloils in routine analysis111. Many private laboratories apply this on-line method since it has clearadvantages over the "manual"off-line methods, despite the need for a sophisticated instrument. With difficult samples and matrices, further characterisation of the MOSH/MOAH fractions can beperformedby using additional analytical techniques, e.g. GC-MS, LC-GC-FID/MS or GCxGC-FID/Ms13,14,15. However the need for further characterisation must be decided on a case by case basisby an experienced analyst. 4.4 Outline of the analytical approach As a general recommendation, the methods published by Kantonales Labor Zurich and BfR6,9,11 can befollowed for determination of the MOSH/MOAH content in food and FCM. Also other approaches,complying with the performance requirements as defined in section 4.6 could be applied. In short MOSH and MOAH are extracted from the sample matrix using an organic solvent after theaddition of internal and verification standards. The extract is submitted to isolation and separation ofthe MOSH and MOAH fractions. MOSH and MOAH fractions are separated on a HPLC silica gelcolumn or a glass column filled with silica/AgNOs using e.g. a n-hexane/dichloromethane gradient. ( Th e compendium of the Federal Inst i tute for Risk Assessment (Bf R ) and the Cantonal Lab o ratory of Zurich (KLZH) (2012)“Determination of mineral oil II h I ydrocarbons SB in foo da ndpackagin g m a terial". ht t ps:/ /www. b fr.b u nd.de/c m / 3 43/ me s s ung- von - mineral oel-kohlenwasserstoffen-in -l ebensmit t eln-u n d-ve r packungsm a teri a l i en . pdf ) ( "Biedermann M, Munoz C, Grob K. (2017) J Chrom.A 1521, 140 ) ( Spack L., Leszczyk G . , Varela J., Simian H., Gude T., Stadle r R. (2017) Food Additive s & Contaminants: Part A 34(6), 1052 ) ( Po p ulin T., Biedermann M., Gr o b K., Moret S., Conte L. (2004) Food Additives and Con t aminants 21(9), 893 ) Each fraction is transferred in large volume either on-line or off-line to a GC pre-column. Solventvapours are discharged via a solvent vapour exit located between the uncoated pre-column and theGC separation column or by using a solvent vent in a PTV injector. Volatile components are retainedby solvent trapping applying a partially concurrent eluent evaporation. High boiling components,spread over the entire length of the flooded zone, are refocused by the retention gap technique. The signal area in the FID chromatogram attributed to MOSH/MOAH is calculated by integration ofthe chromatogram covering the range of en-C10 to
还剩34页未读,是否继续阅读?
继续免费阅读全文产品配置单
GERSTEL(哲斯泰)为您提供《食品和食品包装中矿物油污染( MOSH & MOAH )检测方案(自动进样器)》,该方案主要用于其他食品中环境污染物检测,参考标准《暂无》,《食品和食品包装中矿物油污染( MOSH & MOAH )检测方案(自动进样器)》用到的仪器有GERSTEL LabWorks 平台。
我要纠错相关方案