最新刊期
卷 41 ， 期 10 ， 2022
- 摘要：A method was established for the discrimination of recycled and virgin polyethylene terephthalate（PET） by head-space solid phase microextraction/comprehensive two-dimensional gas chromatography－quadrupole time-of-flight mass spectrometry（HS－SPME/GC × GC－Q－TOF MS） combined with chemometrics．Firstly，volatile organic compounds（VOCs） of recycled and virgin PET were detected to obtain their peak area data for building discrimination datasets. Then the markers and high-level markers were selected on the basis of orthogonal partial least squares discrimination analysis（OPLS－DA） and T-test．The principal component analysis（PCA） and linear discrimination analysis（LDA） models based on all compounds，markers and high-level markers were established．The results showed that PCA model could well explain the differences between recycled and virgin groups，while the accuracies for calibration and validation sets reached 100% and 97.1% respectively in LDA model．This study indicated that the approach above was accessible，high stable and predictable．Besides，a total of 468 VOCs were detected and identified，of which 31 VOCs were classified as high-level markers．The possible origins of these high-level markers could be food，medicine，cosmetics，pesticides，plastic，industry and unknown sources.关键词：HS－SPME;GC × GC;Q－TOF MS;chemometrics;polyethylene terephthalate;recycled plastics;volatile organic compound
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发布时间：2023-01-04 - 摘要：Headspace/gas chromatography－mass spectrometry（HS/GC－MS） combined with MS－DIAL software was applied to the detection of volatile organic compounds（VOCs） in 19 commercial plastic composite packaging bags after 60Co-γ irradiation（0－10 kGy） to address the problem of unknown irradiation products generated by sterilization of plastic packaging．The deconvolution，peak alignment and substance characterization results of the spectra were analyzed by MS－DIAL software，and the VOCs composition of the materials before and after irradiation was analyzed by orthogonal partial least squares－discriminant analysis（OPLS－DA） model to examine the changes of VOCs composition in the composite packaging materials under different irradiation doses．The results showed that the VOCs in the composite packaging were mainly alkane and alkene，while the composition of VOCs in the composite packaging before and after 60Co-γ irradiation was significantly different，and the total amount of VOCs produced by the packaging increased with the irradiation dose．Through the analysis of the importance of projection variable（VIP） value in OPLS－DA model，17 substances with significant contribution to the difference were selected. Most of these substances were degradation products of materials，and the detected amount showed an increasing trend with the irradiation dose．The results of the study provide a basis for the development of a database for volatile unintentionally added substances in irradiated packaging.关键词：plastic composite packaging materials;volatile organic compounds（VOCs）;chemometrics;headspace/gas chromatography－mass spectrometry（HS/GC－MS）
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发布时间：2023-01-04 - 摘要：The color and overall migration of recycled polyethylene（PE） films containing different proportion of scraps were determined．The volatile substances were screened by gas chromatography－mass spectrometry（GC－MS），and the different substances were analyzed by chemometrics．The experimental results showed that the addition of scraps exerted a negligible effect on the color of the single-layer recycled film，while the total migration of the virgin and recycled PE films in four food simulants was less than the safety limit of 10 mg/dm2．A total of 90 volatile organic compounds were detected by GC－MS，mainly including aliphatic hydrocarbons，additives and their degradation products and impurities．The recycled PE films were divided into three categories by using principal components analysis（PCA） and orthogonal partial least squares－discriminate analysis（OPLS－DA） models．The recycled PE films were similar to the original film when the contents of scrap were lower than 10%．Further evaluation was needed when the contents of scrap were between 10% and 50%，and more attention was needed at higher than 50%．Moreover，V－plot was constructed to screen 26 characteristic components that caused the sample differences，mainly aliphatic hydrocarbons，followed by additives and their degradation products，such as the degradation products of dodecanamide，nonanal and antioxidant 1010．This study provided a reference for the application of “film to film” recycling of food contact scraps.关键词：scrap;recycled polyethylene;gas chromatography－mass spectrometry（GC－MS）;chemometrics
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发布时间：2023-01-04 - 摘要：Based on the European Union regulations，paper straw samples were soaked in the two food simulants. Potential migrants in paper straws were untargeted screened by ultrahigh performance liquid chromatography coupled to quadrupole time－of－flight mass spectrometry（UPLC－Q－TOF MS）．Thirty-one kinds of intentionally or non-intentionally added substances including lubricants，sizing agents，antioxidant degradation products and defoaming agents were screened out. Based on the risk matrix developed by our previous study，namely，risk = hazard （toxicity level + Cramer level + 4 × mutagenicity） × exposure （4 × water solubility + 4 × permeability），the risk of thirty-one kinds of migrants in paper straws were evaluated. The result showed that no grade Ⅰ risk substances were found，and components scored higher in grade Ⅱ risk substances were from several lubricants（such as hexadecenoic acid amide），sizing agents （such as pimaric acid） and defoaming agents（such as polyethylene glycol）．Through semi quantitative analysis on grade Ⅱ risk substances，as well as comparison of exposure and TTC threshold，it is found that amide lubricants have health risks，（especially erucamide） which should be paid attention to in the production and processing of paper straws．关键词：paper straw;food contact materials;ultrahigh performance liquid chromatography coupled to quadrupole time－of－flight mass spectrometry（UPLC－Q－TOF MS）;non-targeted screening;risk matrix
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发布时间：2023-01-04 - 摘要：A method for the determination of the migration of six cyclosiloxanes（D4－D9） to 50% ethanol，95% ethanol and isooctane in food contact silicone rubber products was developed based on gas chromatography－tandem mass spectrometry（GC－MS/MS），which was applied to the determination of 38 actual samples．2 mL of n-hexane was used to extract D4－D9 from 10 mL of 50% ethanol obtained from the migration test¸ followed by filtration and detection．Meanwhile，the 95% ethanol and isooctane were simply determined after filtration．The analysis was carried out in multiple reaction monitoring mode using an HP－5 MS column for separation．The results showed that there were good linear relationships for D4－D9 in the range of 0.05－1.00 mg/L or 0.20－5.00 mg/L，with correlation coefficients（r2） not less than 0.996 0．The limits of detection and limits of quantitation for each target were in the range of 0.02－0.07 mg/L and 0.05－0.20 mg/L，respectively．The recoveries ranged from 90.1% to 106%，with relative standard deviations not more than 13%．The method was used to determine the migration of D4－D9 in commercially available food contact silicone rubber products，and it was found that there was a migration risk of D4－D9 to 50% ethanol，while the migration risk of D4－D9 to 95% ethanol and isooctane was the highest as the detection rate for D4－D9 was 80%．The detection rate for the third migration of D4－D9 to 95% ethanol and isooctane was significantly greater than that for the first migration，while the detection rates for the first migration and the third migration to 50% ethanol were not significantly different.关键词：food contact silicone rubber;cyclosiloxane;food simulant;migration;gas chromatography－tandem mass spectrometry（GC－MS/MS）
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发布时间：2023-01-04 - 摘要：The cyclic oligomers may migrate from polyethylene terephthalate（PET） and polybutylene terephthalate（PBT） coating of metal cans to foods，which may do harm to the human health．Hence，a method was developed for the detection of migration content of PBT/PET cyclic oligomers in coating of metal cans by ultra-high performance liquid chromatography－quadrupole time-of-flight mass spectrometry（UPLC－QTOF MS）．According to the database of food consumption，the surface to volume（S/V） data of food contact materials and the migration tests of PET and PBT cyclic oligomers，the total intake of PET and PBT cyclic oligomers in chinese people exposing to coating of metal cans（fruit cans，drinks cans and beer cans） was estimated，and its risk was assessed by threshold of toxicological concern．Six kinds of PET and PBT cyclic oligomers belonged to the substances of Cramer Ⅲ．The maximum dietary exposure contents of PET and PBT cyclic oligomers were both 1.234 µg/kg·BW/d，which were lower than 1.5 µg/kg·BW/d，the threshold of substances of Cramer Ⅲ．As a result，the intake health risk of PET and PBT cyclic oligomers exposing on coating of metal cans（fruit cans，drinks cans and beer cans） was low，which required no undue attention.关键词：polyethylene terephthalate（PET）;polybutylene terephthalate（PBT）;cyclic oligomers;polymer-laminated metal cans;migration test;threshold of toxicological concern（TTC）;risk assessment
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发布时间：2023-01-04 - 摘要：Faced with the increasingly perfect health standard system for food contact materials，this paper has implemented the proficiency testing（PT） for the determination of potassium permanganate consumption in food contact plastic materials，in order to master the technical requirements for the determination of potassium permanganate consumption，conducting the corresponding compliance judgments and giving full play to the role of proficiency testing for technical ability supervision and quality improvement of inspection and testing institutions．The brown plastic packaging bottles used in food were customized as relevant proficiency testing samples．The homogeneity and stability were evaluated according to the requirements of relevant standards，and robust statistical techniques were used for the collected results．The assigned value and the standard deviation of the performance assessment were determined by Algorithm A，and the influencing factors that may lead to unsatisfactory results were analyzed．There are 192 participating laboratories in this proficiency test，of which 179 obtained satisfactory results，with a satisfaction rate of 93.2%，and 12 laboratories got unsatisfactory results，accounting for 6.3%，and 1 laboratory got suspicious results，accounting for 0.5%．This proficiency testing activity contributed to PT provider a certain understanding of the testing level of laboratories in this field．The overall results presented by the laboratories were satifactory，while the reason for unqualified results of individual laboratories could be analyzed through this proficiency testing so as to achieve the purpose of improving the detection capability.关键词：food contact materials;potassium permanganate consumption;proficiency testing;statistic analysis
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发布时间：2023-01-04 - 摘要：Untargeted screening of semi-volatile compounds in three water-borne coatings was conducted by using gas chromatography－mass spectrometer（GC－MS）．Combined with retention time and NIST mass database，unknown chemicals extracted with methanol under the ultrasonic were deconvolved and determined via MS－DIAL software．63 semi-volatile compounds were tentatively identified，including aromatic hydrocarbons，carbonyl compounds and ester compounds．To highlight the chemicals of concern，substances with similar structures were quantified by external standard method．The results showed that，polymerization monomers，including 2-ethylhexyl acrylate，isooctyl acrylate and 2-ethylhexanol methacrylate were found in three water-borne coating samples．Meanwhile，added additives of different concentrations，such as ethanol，2-［2-（2-butoxyethoxy）ethoxy］-，2， 4， 7， 9-tetramethyl-5-decyne-4， 7-diol as well as potential non-intentionally added substances（NIAS），such as 2-ethylhexanol，dodecanol，dibutyl phthalate，were detected in the coating samples. Furthermore，to elucidate the potential risk source of water-borne coatings，their multiple toxicity endpoints of acute toxicity，developmental toxicity，mutagenicity，carcinogenicity and Cramer class were evaluated using toxicity estimation software tool（T.E.S.T） and VEGA QSAR．It could be found that the safety risks of water-borne coatings mainly originate from Cl，N or Si element-contained NIAS，and substances of high concern，e.g.，2-ethylhexanol，styrene and 2-ethylhexyl acrylate，while other intentionally added substances（IAS） are relatively much safer.关键词：water-borne coating;gas chromatography－mass spectrometry（GC－MS）;untargeted screening;hazard assessment
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发布时间：2023-01-04 - 摘要：An ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with salting-out assisted liquid－liquid extraction（SALLE） was established for the simultaneous determination of 12 phthalate esters in milk beverage．The sample was firstly extracted with acetonitrile，then salted out with（NH4）2SO4 and separated on a phenyl column，and finally analyzed by electrospray tandem mass spectrometry in positive ion and multiple reaction monitoring（MRM） mode．The extraction parameters affecting the SALLE procedure such as kind and volume of extracting solvent，type and amount of salt were optimized．Under the optimal conditions，the method showed a good linearity for 12 phthalate esters in the corresponding mass concentration ranges，with correlation coefficients（r2） not less than 0.997．The detection limits and the quantitation limits for 12 phthalate esters were in the range of 0.03－0.6 μg/kg and 0.1－2.0 μg/kg，respectively．The spiked recoveries for 12 phthalate esters in milk beverage ranged from 70.8% to 111%，with the relative standard deviations of 0.30%－7.2%．The effects of temperature and light on phthalate esters migration from polythylene terephthalate（PET） plastic bottle were investigated．The results showed that the migration level of dibutyl phthalate（DBP） at high temperature（80 ℃） was significantly higher than that under other conditions．With simple operation，low cost and good accuracy，the established method could meet the requirements for monitoring the level of 12 phthalate esters in milk beverage.关键词：milk beverage;phthalate esters;salting-out assisted liquid－liquid extraction;ultra performance liquid chromatography－tandem mass spectrometry
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发布时间：2023-01-04 - 摘要：Unknown species migrating from commercially available disposable plastic tableware（including lunch boxes，cups and straws） to food simulant 10% ethanol or substitute test media 95% ethanol were screened and identified，to assess the safety risk of migrated substances from disposable plastic tableware．Commercially available samples were soaked with 10% ethanol or 95% ethanol under the specific migration conditions according to the usage of the samples．Soaking solutions of products from migration tests were concentrated and determined by gas chromatography－mass spectrometry（GC－MS）．Meanwhile，each sample was analyzed with infrared spectrometer，which indicated that the tested disposable plastic tablewares were mainly made of polylactic acid or polypropylene．MS spectra of migrated species from GC－MS were then compared with a MS database．Combined with material information from infrared spectrometer，structures of migrated species were predicted．Then the structures were confirmed by comparison with reference substances or determination of triple quadrupole MS．Species could further be quantitatively determined with corresponding reference substances．Cramer’s rule was used to predict the toxicity of migrated substances．Combined with the measured migration amount，safety risks of migrated substances and relative samples were assessed．Finally，19 kinds of migrated species in all the tested samples were screened and identified，among which intentionally added substances（IAS） included synthetic raw materials of polylactic acid resin or its blended resin（like lactide，butane-1，4-diol and dimethyl succinate），lubricant（like methyl oleate） and plasticizers（like di（2-ethylhexyl） adipate）．Non-intentionally added substances（NIAS） included oligomers of polyester or silicone resins（like cyclic siloxanes） and by-products from plasticizers or antioxidants additives．There were few kinds of substances migrating out of polypropylene based tableware，while there were relatively more kinds of substances migrating from polylactic acid based tableware or tableware of inorganic filled polypropylene．Most of identified IAS or NIAS，which are structurally hydrophobic，tend to have higher migration in substitute test media 95% ethanol（which is a substitute of fatty food simulant） than the aqueous food simulant 10% ethanol．Since Cramer's rule predicted species like cyclic siloxanes and methyl 3-（3，5-di-tert-butyl-4-hydroxyphenyl） propionate had relatively high toxicity，the safety assessment results suggest that，when disposable plastic tableware is used to contact with fatty food，the migration and hazards of oligomers and by-products of antioxidants in polylactic acid or composite polypropylene tableware need to be paid attention to.关键词：disposable tableware;non-intentionally added substances;gas chromatography－mass spectrometry（GC－MS）;migration
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发布时间：2023-01-04
Scientific Papers
- 摘要：In order to evaluate the migration risk of benzeneseries from food contact materials and products，a purge-and-trap/gas chromatography－mass spectrometry（P&T/GC－MS） was developed for the simultaneous determination of nine benzene compounds in food contact materials and products．Food simulants included 4% acetic acid，10% ethanol and olive oil. 9 kinds of benzeneseries were separated on an HP－INNOWax capillary column，and detected by MS in selected ion monitoring（SIM） mode．Results showed that there were good linear relationships for the analytes in the range of 0.50－5.0 μg/kg or 0.50－5.0 μg/L，with their correlation coefficients（r2） not less than 0.995．The limits of detection and limits of quantitation of the method were 0.15 μg/kg and 0.50 μg/kg，respectively．The recoveries ranged from 78.5% to 107%，with the relative standard deviations（n = 6） of 1.1%－9.2%．With high accuracy and good reproducibility，the established method could be used to determine the migration of nine benzeneseries in food contact materials and their products.关键词：food contact materials and products;purge-and-trap;gas chromatography-mass spectrometry;benzeneseries
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发布时间：2023-01-04 - 摘要：A pyrolysis/gas chromatography－mass spectrometry was established for the determination of alternative brominated flame retardants（ABFRs） in recycled styrene polymers in this paper．And the pyrolysis and chromatography－mass spectrometry conditions were optimized．Samples were crushed into small particles in advance．The 13 ABFRs were pyrolyzed out of polymers by programmed heating in the pyrolysis furnace，then separated on a ZB－5HT INFERNO column（15 m × 0.25 mm × 0.10 µm），and determined by mass spectrometry under selected ion monitoring（SIM） mode．There were linear relationships for the analytes in the range of 10－500 mg/kg，with limits of quantitation between 3.2 mg/kg and 10.5 mg/kg．The recoveries ranged from 85.3% to 114%，with relative standard deviations（RSDs，n = 6） not more than 16%．This method was rapid，precise and convenient to operate，and was appropriate for the determination of ABFRs in recycled styrene polymers．关键词：recycled plastic;styrene polymers;alternative brominated flame retardants;pyrolysis;gas chromatography－mass spectrometry
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发布时间：2023-01-04 - 摘要：A gas chromatography－thermal energy analyzer（GC-TEA） method with alcoholic food simulants was established for the simultaneous determination on the migration amounts of 15 N-nitrosamines in food contact materials and products．The gas chromatographic conditions and pretreatment method（liquid－liquid extraction method） were optimized．Using 10% ethanol，20% ethanol and 50% ethanol as food simulants，the immersion solution was diluted，liquid－liquid extracted and concentrated，then separated on a DB－FFAP column，and finally detected by the thermal energy analyzer and quantified by the external standard method．Under the optimized experimental conditions，good baseline separation for 15 N-nitrosamines was achieved in the linear range of 0.025－0.5 mg/L，with correlation coefficients（r2） greater than 0.998．The limits of detection（LODs） and limits of quantitation（LOQs） were 0.200 μg/kg and 0.625 μg/kg，respectively．The spiked recoveries ranged from 85.7% to 106%，with relative standard deviations（RSDs） less than 10%．With the advantages of simple operation，good linear range，high sensitivity and accuracy，the method was suitable for the determination of 15 N-nitrosamines in food contact materials and products．关键词：food contact materials and products;N-nitrosamines;alcoholic food simulants;specific migration amounts;gas chromatography－thermal energy analyzer（GC－TEA）
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发布时间：2023-01-04 - 摘要：An ultra-high performance liquid chromatography－orbitrap high resolution mass spectrometric（UPLC－Orbitrap HRMS） method was established for the determination of 23 organic antibacterial agents，including 4 parabens and 19 chlorophenols in food contact paper products．The samples were ultrasonically extracted with methanol as extraction solvent，then centrifuged，concentrated and fixed volume by nitrogen blowing，filtered by 0.22 μm membrane，and finally analyzed by UPLC－Orbitrap HRMS．The separation was performed on a Waters Atlantis T3 （150 mm × 2.1 mm，3 μm） by gradient elution，using methanol－5 mmol/L ammonium acetate containing 0.4% acetic acid as mobile phase．Electrospray ionization（ESI-） mode was used for ionization，and full MS/dd－MS2 scanning mode for MS．Retention time and secondary subion MS spectrum were used for qualitative analysis，and chromatography peak area of extracted ions was quantified．The limits of quantitation for parabens and chlorophenols were 0.05 μg/kg and 0.05 mg/kg，respectively，and the linear relationships were good in the ranges of 0.05－5.0 ng/mL and 0.05－5.0 μg/mL，respectively，with correlation coefficients greater than 0.997．The average recoveries for blank matrix samples at three spiked concentrations ranged from 81.7% to 119%，with relative standard deviations of 2.0%－8.8%．The method is convenient and efficient，and could be used for screening and confirmation of organic antibacterial agents in food contact paper.关键词：food contact paper products;organic antibacterial agent;chlorophenols;parabens;ultra-high performance liquid chromatography－orbitrap high resolution mass spectrometry（UPLC－Orbitrap HRMS）
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发布时间：2023-01-04 - 摘要：An analytical method for migration amount of ethyleneimine in food contact paper and paper product was established by ultra-high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．Formic acid aqueous solution（0.1%，volume fraction） and methanol were adopted as mobile phases，electrospray ionization（ESI） ion source was used to ionize the target，and multi-reaction monitoring mode was ultilized for detection．The results showed that there was good linear relationships for ethyleneimine in simulants of 4% acetic acid，10% ethanol，95% ethanol and isooctane in the mass concentration range of 0.003－0.05 mg/L，with the detection limits of 1 μg/L．Meanwhile，good linear relationship for ethyleneimine in simulant of olive oil existed in the range of 0.003－0.05 mg/kg，with a detection limit of 1 μg/kg．The spiked recoveries ranged from 96.0% to 102%，with the relative standard deviations（RSDs） of 1.6%－5.9%．20 batches of samples were selected for practical detection，of which 2 batches were found to contain ethyleneimine．The method was sensitive and accurate，and it was suitable for the determination of migration of ethyleneimine in food contact paper and paper products.关键词：ethyleneimine;migration;food contact material;ultra-high performance liquid chromatography－tandem mass spectrometry
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发布时间：2023-01-04
Experimental Techniques and Methods
- 摘要：As a potential risk to food safety，chemical migration from food contact materials（FCM） is attracting growing interest in the last decades，which promotes the development of analytical techniques. Conventional target analyses mainly focus on some intentionally added substances（IAS） and few non-intentionally added substances（NIAS），which are therefore incapable of screening other potentially present substances. In contrast，untargeted screening analysis covers all detectable substances，providing chemical information derived from FCM as comprehensive as possible，which is fundamental for the risk assessment，legislation，and risk management of FCM. However，challenges remain in untargeted screening analysis of FCM nowadays. This work provides an overview on untargeted screening technology used in FCM with a focus on chemical extraction and identification on FCM. The potential of mass spectrum libraries is highlighted，especially publically available libraries，high resolution mass spectrometry，open-source tools，chemical databases pertinent to FCM，as well as retention index and collision cross section（CCS） predictions，etc.，in the qualification of substances derived from FCM. The work is also helpful to ultilize various resources and tools to facilitate untargeted screening analysis in the field of FCM.关键词：food contact materials;untargeted screening;qualitative analysis;data processing;high resolution mass spectrometry
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发布时间：2023-01-04 - 摘要：With the increasing pollution of plastic waste，the recycling of plastic has attracted much attention．Food contact materials have become an important object of plastic recycling，but the non-intentionally added substances（NIAS） in recycled plastics are a major difficulty for their ultilization in food contact materials．In order to avoid the recycled plastics that do not meet regulations appearing in food contact materials market and endangering the health and safety of consumers，the discrimination technology for recycled plastics is very essential．Research on NIAS in recycled plastics and the discrimination of virgin and recycled plastics at home and abroad is summarized in this paper．At present，the main discrimination methods for recycled plastics mainly include mass spectrometry，spectroscopy and thermal analysis technology．In recent years，chemometrics has gradually been used in the discrimination on recycled plastics，which improves the efficiency and accuracy of discrimination.关键词：recycled plastics;non-intentionally added substances;mass spectrometry;spectroscopy;thermoanalysis technology;chemometrics;discrimination
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发布时间：2023-01-04
Reviews
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