已知和未知食品接触材料中鉴定检测方案(液质联用仪)

ThermoSCIENTIFIC METHODS FOR IDENTIFICATION OF KNOWN AND UNKNOWN FOODCONTACT MATERIALS BY MEANS OF HPLC-HIGH RESOLUTION-ACCURATE MASS SPECTROMETRY Laszlo Hollosi and Michal Godula Food Safety Response Center -Thermo Fisher Scientific， Dreieich， Germany Packagingmaterials (PM) and non-intentionally added substances (NIAS) arecurrently one of the hottest research topicsin food safety relevant applications.Currentresearch especially TOcuses onidentification of non-expected or up-to-nowunknown compounds. Recent poster aimss to present suchapproaches supported by High-Resolution MS(HRMS) basedLC-MSmethods forr identification ofknownauthorized or unauthorized substances.We demonstrate the power of HRMS andTraceFinder 3.1 software with known andunknown compounds. ANALYTICAL METHODOLOGY 1) Establishment of database (DB)with High-Resolution m/z data 2) Performing analyticalmeasurement -direct analysis by FIA-HRMS-LC-HRMS (after extraction) 3) Data mining， evaluation oo INSTRUMENTATION Thermo Fisher Scientific Exactive TM OrbitrapTMhigh-resolution benchtop mass spectrometercoupled to Transcend TLX-1 system.Column： Hypersil Gold C8 HPLC， 100x2.1 mm，3 pm. Mobile phase： A： MeOH， B： water.Gradient run： 0-1 min： 50%A， 1-6 min ramp to100%A and hold for 4 min. Flow： 0.4 ml/min. HR-MS settings： R=100，000；lonisation mode： ESI and APCIboth in positive/negative； Mass range： 60 -600m/z； Maximum injection time： 500ms：Fragmentation method： HCD， Sheath gas： 40；AUX gas： 5； Vaporiser temperature： 350℃；Capillary temperature： 300°℃. Targeted screening for known and unknowncompounds Database establishment Figure 1. TraceFinder 3.1 database compounddefinition page with precursor and fragment nmasses. 980 Figure 2. Fragmentation profile for 2，5-bis(5-tert-buthyl-2-benzoxaolyl)thiophene with a， Ecoll=0 kV and b) Ecoll=60 kV. ldentification of known compounds Identification was conducted both byTraceFinder 3.1 quantitative and screeningmethods. Fragment iionswere usedforconfirmation. Figure 3. Identification of 2，5-bis(5-tert-buthyl-2-benzoxaolyl)thiophene in TraceFinder result page forquantitative methods. Identification was conducted both by TraceFinder3.1 screening and quantitative methods based onthe established database search. Extracted ionchromatograms(XIC) were identified andcompared to FIA observed or online availablespectral fingerprints. Spectra were recorded inboth ESl and APCI ionisation mode. Figure 4. APCI screening method result withcompound prediction for an unknown compound. 2，5-bis(5-tert-buthyl-2-benzoxaolyl)thiopheneand 2-hydroxy-benzophenone were used asknown model compound for testing and fourindividual unknown compounds were receivedfrom co-operation partner for demonstration ofidentification process. Thermo Fisher ScientificTraceFinder 3.1 softwarewas usedforevaluation.Accurate mass database was established for600 potential target： compounds. HRMSprecursor and fragment masses were identifiedfor known compounds in LC-HRMSexperiments.0M 125Ma朗2.5-bis-(5-tert-buthyl-2-benzoxazolyl)thiophene inasmm2，4-dihydroxy-benzophenone2-hydroxy-4-octyloxybenzene品CHO CHO0005f979Erucamid水羽051001255101094253： 33lethyV/ethyl/buthyl m etacrylate 瞿明 声 copolymerii Figure 5. Quick overview of possible target compoundidentity in quantitative method result window (APCIionisation). Identified unknown compounds Figure 6. Overview of the identified four unknowncompounds. SUMMARY>All test compounds could be identified correctly > HRMS is essential for high confidentialidentification of both known and unknowncompounds > adequate software support with correctdatabases is necessary to apply in order to getcorrect results. 装材料 (PM) 和非有意添加物质 (NIAS) 是当前食品安全相关应用中最热门的研究课题之一。当前研究特别关注鉴定非预期或目前尚属未知的化合物。