Thermo Scientific GC and GCMS Systems Analysis of
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Thermo Scientific GC and GC-MS Systems Analysis of chemical contamination in nutraceuticals and other matrices.
Gas Chromatography Products Trace 1300/1310 ISQ Gas Chromatograph Single Quadrupole GC-MS TSQ 8000 ITQ Ion Trap GC-MS/MS 2 Triple Quadrupole GC-MS/MS
TRACE 1300 Series Gas Chromatograph Launched at Pitt. Con March 12
TRACE 1300 Series – Two Systems Available TRACE 1310 4 TRACE 1300
Expand throughput with flexible automation TRACE 1300 series GC is part of the Thermo Scientific GC/MS solutions Tri. Plus RSH: Liquid, Headspace and SPME injections in a single sequence, with unattended syringe switching Sample preparation capabilities, without increasing the bench space 5
TRACE 1300 Series: Tailor instrument configuration • Modules are user installable in only two minutes • just removing three screws you’ll put the new module in place • No special training, dedicated tools or on-site service engineers required 6
USP 467 Analysis using the TRACE 1310 • Triplus RSH • Dilute • Headspace • Liquid injection • TRACE 1310 GC • Split/splitless injector • TR-V 1 column • FID detector 7
USP 467 Analysis using the TRACE 1310 1_ methanol 2_ acetonitrile 3_dichloromethane 4_trans-1, 2 -dichloroethane 5_cis-1, 2 -dichloroethane 6_tetrahydrofuran 7_cyclohexane 8 - methylcyclohexane 9_ 1, 4 -dioxane 10_toluene 11_chlorobenzene 12_ethyl benzene 13_ m-xylene/p-xylene 14_ o-xylene dichloromethane R 2 = 0. 9994 25000000 R 2 = 0. 9999 20000000 peak area 15000000 10000000 5000000 0 0 0 8 tetrahydrofuran 100 200 300 400 conc (ppm) 500 600 700 0 200 400 conc (ppm) 600 800
ISQ Single Quadrupole GC-MS
ISQ: Features • Dual Filament assembly • ISQ Ion Path 10 • Ion Source
Full Scan/SIM Methodology for Drinking Water 11
Source Maintenance without Breaking Vacuum Step 2. Remove source Step 1. Insert removal tool Step 3. Hot source is held in tool 13 Step 4. Push source out of tool
ITQ Ion Trap GC-MS/MS
Why an ion trap and MS/MS? Gamma BHC Methiocarb Mevinphos Single Quadrupole – SIM Mode at 5 ppb Gamma BHC Methiocarb Ion Trap – MS/MS Mode at 5 ppb 15 Mevinphos
Multi-Residue Pesticide Analysis in Tea ITQ Ion Trap GC-MS/MS • Split/splitless injector, 250 °C, 2 µL inj. • Surge pressure 250 k. Pa, 30 s • Low Endrin/DDT breakdown • TRACE™ TR-Pesticide • 35% diphenyl/65% dimethyl polysiloxane • 30 m x 0. 25 mm x 0. 25 μm w/ 5 m guard column • 1 m. L/min, const. Flow 16
ITQ Chromatograms in MS/MS and Full Scan GC-MS/MS • Interference free quantitation by MS/MS • Unknown peak investigation by Full Scan 17 GC-Full Scan-MS
Analysis of Phthalates in Serum The Problem: EI GC-MS analysis of phthalates generates a non-specific full-scan spectrum with prominent m/z 149, and not many other identifying ions The Solution: PCI with ammonia generates a prominent [M+1] at m/z 391, perfect for MSn analysis for improved specificity and confidentification & quantitation 18
Results – All Work Done in Serum Calibration curve 1 to 10 µM DEHP in serum Results from sample 5. 3 µM DEHP in serum 19
TSQ 8000 Triple Quadrupole GC-MS/MS Launched at ASMS May 20
Achieve Low Detection Limits With Confidence Malathion extract at 5 ppb • Cut through chemical background • High selectivity in matrix compared with single stage MS • Selected Reaction Monitoring (SRM) SIM SRM 21 • High precision at low concentrations • Femtogram level detection • Confirming ions
Not Just MS/MS Performance Full Scan SIM • High full scan spectral quality • Searchable with NIST etc. • High sensitivity SIM & Full Scan • Virtually indistinguishable from a single quad instrument • Dual acquisition modes • Quan & qual in the same run Lindane isomers 40 ppb in cucumber in simultaneous full scan/SIM 22
Designed For More Uptime, More Results Reported • Design based on strong reputation • Thermo Scientific ISQ Single Quadrupole GC-MS • Innovative GC modularity • Thermo Scientific TRACE 1300 Series GC • Optimized maintenance 23 Before EU limit for LOQ %RSD • Routine-grade robustness • Extracta. Brite ion sourceno-vent maintenance • Heated sample path zones for reduced ion burn %RSD pesticides (10 ppb) before and after 1, 400 vegetable matrix injections After EU limit for LOQ
SRM Enables Optimized Sample Preparation 1, 3 –dichlorobenzene 1, 4 dichlorobenzene and 1, 2 dichlorobenzene (left to right) in ASE soil extract at 5 ppb. • Explore generic sample approaches • Method consolidation • Eg. Qu. ECh. ERS • Reduce number of steps • Pre-concentration • Clean-up • Bring sample preparation onboard TSQ 8000 • Tri. Plus RSH autosampler 24
Consolidated, Faster Methods With More Compounds • Method consolidation • Combine separate MS analyses • Driven by selectivity of SRM • Faster run times • Compress chromatography • Using MS/MS resolution • Clean peak detection • Less manual integration changes • Fast data processing 25 Real example of method consolidation on the TSQ 8000. Five SIM methods combined to form a powerful MRM method for 350 pesticides (700 transitions)
26 SRM Optimization Auto. SRM Method Sync A Fast, Simple Route to High Performance MS/MS Inst. Method TSQ 8000 Thermo Scientific Trace. Finder SW Unknown SRM Transitions • The very beginning • or a SIM Method Known SRM Transitions • From an existing method • or SRM Transition list Optimized SRM Transitions • From Compound Data Store • or existing TSQ 8000 method • SRM management tools • SRM creation and method management independent of your starting point
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