Presentation on theme: "Flavor and Odor Analysis in Foods and Food Packaging"— Presentation transcript:
1Flavor and Odor Analysis in Foods and Food Packaging
2Presentation Overview Introduction to Large Volume Static Headspace (LVSH) TechniqueAdvantages of LVSH/GC(MS)Analytical ProcedureExamples of Food Products AnalyzedFood Quality Determination by LVSHSummary
3GC/MS Detection Limits vs Headspace Sample Volume 10001001010.10.0110-310-410-5LoopPreconcentrationPPMLODVol vs Conc.MINIMUM VOLUME REQUIRED (CC)
4Large Volume Headspace Requires Preconcentration HP 5973 GCMS Volume ReductionLarge VolumeInlet or Autosampler
5Large Volume Static Headspace Autosampler Introduces cc of headspace to the 7100 PreconcentratorAccommodates solids and liquidsDetection limits 100x lower than conventional loop injection headspace“See what you can smell”
6LVSH Sample Platforms and Enclosures Samples are placed in disposable vials, reducing potential for contamination of sample platforms.Sample Platforms use quick connects, simplifying removal for oven bakeout.
7Advantages of Large Volume Static Headspace (LVSH) Cleaner. No aerosols or foaming to contaminate sample transfer linesLarger Sample LoadingLow detection limits without sample heating.Less chance of producing artifacts.Sample remains in natural state.Ideal for kinetic / aging studiesOutgassing ratesEffects of Atmosphere and Storage TemperatureBetter recovery of reactive compoundsStrong carbon based adsorbents are avoidedInert, Silonite tubing used throughoutNo sample fractionation (SPME)
8Food and Beverage Analysis by Large Volume Static Headspace (LVSH) / GCMS Analysis HP 5973 GCMS LStage Preconcentrator7032L 21-Position LVSH/MiniCan AutosamplerMulti-Channel Standards Diluter
13Silonite Tubing VOC Adsorption/Absorption Study Less adsorption of Diethylbenzene on Silonite tubing. No deactivation needed.Faster sample equilibration with tubing surface.Less potential for carryover.RESPONSiloniteBrand BDeact. Brand BFlush Time (Min.)
147100 Water and CO2 Management Techniques MFCPUMPH2OPost-Injection BakeoutHelium CarrierHeliumToGCFocuserGlass BeadsTenaxSampleInternalStandardCalibrationStandardCryogen in
153-Stage Flexibility for GCMS Analysis of Multiple Sample Types and Matrices Sample Type Mode Trap Trap2Trap 3 - On-column focuser for capillary GC/MS
16Improper Water Management 400cc VOC STD, Full Scan 15-270 amu
17Vinyl Chloride 100x Calibration Curve using Variable Volume / Single Standard Calibration
18Fast Injection and Proper Water Management Minimizes Tailing of Polar VOCs Column: HP1, 60m, 0.32mm ID, 1um film.Flow rate: 1.5 ccmCarrier: He
19Advantages of 7100 Multi-Stage Preconcentration Multiple Preconcentration Options Depending on Target Compounds and Matrix (CO2, ETOH)Reduced Temperature Trapping Minimizes Sample Stress, Maximizing Recovery of Thermally Labile Flavor and Odor CompoundsSilonite Tubing Creates an Extremely Inert Sample Flow Path to Further Improve RecoveryDemonstrated Recovery of Sulfur and Nitrogen Compounds
24Using LVSH to Determine Product Quality Markers in Fruits and Vegetables Analysis of 100cc of Headspace allows detection of VOCs indicating condition of food products.Monitoring changes in VOC ratios as food spoils allows quantitative evaluation of extent of spoilage.Once specific “Markers” are determined, remote headspace techniques can be used to predict food condition and time until spoilage in storage containers and warehouses.
26LVSH Analysis of Grapes - Scaled to show PPB Cmpds (Loop Injection Detection Limit)ISIS11. EthylAcetate2.Limonene221
27LVSH Analysis of Grapes Ethyl Acetate concentration increases as grapes age, while naturally occurring Limonene drops off.The ratio of EA/Limonene is a good indicator of product qualityAcetaldehyde, a non-desirable component in wine, is present even before the fermentation process begins.
29LVSH Analysis of Lettuce Ethanol, Dimethyl Sulfide, and Acetaldehyde show large increases as lettuce spoilsNaturally Occurring Limonene drops in concentrationThe ratio of DMS to Limonene was a good indication of freshness
31LVSH Analysis of Tomatoes - Scaled to show PPB Cmpds MultiplePPB LevelMarkers
32LVSH Analysis of Tomatoes Heavy aldehydes increased as food spoilsThe largest increase was from a semi-volatile tentatively identified as DHHNIn this study, the ratio of DHHN to 2-Methyl Furan was determined to be an excellent indicator of product quality
33Chocolate vs Carob Peanuts by LVSH/GCMS HexanalChocolate Peanuts100cc, LVSH60m, HP1, 0.32mm ID, 1um7032LVSH/7100/5973HexanalCarob Peanuts100cc, LVSH60m, HP1, 0.32mm ID, 1um7032LVSH/7100/5973
34Whole Garlic vs Garlic Powder by LVSH/GCMS 100cc, LVSH60m, HP1, 0.32mm ID, 1um7032LVSH/7100/5973Garlic Powder100cc, LVSH60m, HP1, 0.32mm ID, 1um7032LVSH/7100/5973
36MiniCan Samplers Allow Direct Sampling of Gas Phase Flavors and Odor Compounds Collection of Remote Headspace Samples Improves Monitoring Effeciency.MiniCan Samplers are SiloniteTM Coated to reduce surface losses.Monitor Process Streams, Holding Tanks, Reactors, etc.
42Support for R&D and QAFully Characterize Products down to Olfactory Detection LimitsIdentify Good and Bad “Markers” in product or packagingMonitoring on-line (Sequence Looping)Monitoring at-line (Sampling Ports)Solids, Liquids by LVSHGases by MiniCan Samplers
43ConclusionLarge Volume Static Headspace (LVSH) is a new analytical tool available to food and beverage Chemists which enhances the detection of headspace components using GC and GCMS analysis.Maintaining the sample in a more natural state allows the analysis of “normally occurring” odor and flavor compounds.Inert flow paths and reduced temperature trapping increases the range of analytes that can be recovered, including oxygen, nitrogen, and sulfur containing compounds.