Meeting the Challenges in the Field of Food Control

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1 Meeting the Challenges in the Field of Food Control Jutta Guggenberger-Brunner Sales Waters Austria

2 Trends in Global Food Rising Global Demand Shifts in Production Markets Tougher Global Competition Increasing Global Legislation

3 Analytical Technology Veterinary drug and pesticide testing Tandem quadrupole MS/MS is dominant Both GC and LC; but increasingly LC/MS/MS Much interest in multi-residue methods New trend towards accurate mass techniques (eg. ToF/MS) Used for screening and confirmation of targeted analytes Mass accuracy and medium resolution are required to avoid false results Some substances, eg. Mycotoxins, often still use fairly simple approaches: TLC, LC, IAC/FL(LC), ELISA etc.

4 Increase the Productivity % UPLC- MS/MS HPLC- MS/MS Time

5 UPLC Throughput HPLC: Total run time 5.5 min XTerra MS C x 50 mm, 3.5 µm 0.3 ml/min UPLC: Total run time 1.5 min ACQUITY UPLC BEH C x 50 mm, 1.7 µm 0.6 ml/min Validated assay for risperidone/9-hydroxyrisperidone in human plasma 2mM aq. NH 4 OAc (ph 9.0) / methanol gradient 3x improvement in LOQ >3x improvement in run time

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7 Customer Needs and Waters Design 2006 Customer Needs A fully integrated ACQUITY UPLC/MS/MS system Faster data acquisition rates required for UPLC compatibility Instrumentation that is more accessible 2006 Waters introduced TQ Detector Highest level of MS-UPLC system integration seen to date T-Wave collision cell technology New IntelliStart (Highly automated operation)

8 Customer Needs and Waters Design 2008 Customer Needs UPLC/MS/MS with greater sensitivity than TQD High performance MS/MS that is simple to operate More information rich data for extra confidence in your Quantitative assays Service a broader range of applications 2008 Waters introduced Xevo TQ Higher sensitivity, especially at UPLC flow rates IntelliStart, first time on a high performance MS New ScanWave collision cell technology New universal ion source architecture

9 Customer Needs and Waters Design 2010 Customer Needs Detection of banned substances easier Monitoring of low exposure drugs or drinking water analysis easier Blood spot analysis easier It possible to work with small sample volumnes It possible to reduce matrix effects by simple sample dilution 2010 Waters introduced Xevo TQ-S Higher sensitivity than Xevo TQ Introducing StepWave Technology New Software tools for calculating Matrix Effects

10 Waters TQ MS Portfolio Xevo TQ-S Enhanced sensitivity StepWave TM ion optics TQ Detector Entry level TQ Fast data acquisition Routine UPLC-MS/MS Xevo TQ More sensitive than TQD Fast data acquisition ScanWave Enhanced product ion scanning RADAR acquisition mode Universal ion source architecture

11 XEVO Family of Mass Spectrometers Tandem Quadrupole Quadrupole Time of Flight Accurately measure the concentration of target compounds present at very low levels in complex samples Comprehensively identify & quantify compounds with exact mass in complex samples XEVO TQ XEVO TQ-S XEVO QTof XEVO G2 QTof

12 Class leading UPLC MS/MS performance Xevo TQ-S Larger sampling orifice

13 Class leading UPLC MS/MS performance Off-Axis design Narrow Ion Tunnel Conjoined to Wide Ion Tunnel Maximising signal Minimising noise

14 Relative ion abundance % % Increased Sensitivity Xevo TQ-S Enhanced sensitivity Reserpine (50fg) UPLC/MRM, ESI + >25X increase in peak area >5X increase in signal:noise Xevo TQ Time Time

15 Relative ion abundance % % Increased Sensitivity 100 Xevo TQ-S Enhanced sensitivity Desompressin (Peptide) UPLC/MRM, ESI+ 129X increase in peak area 25X increase in signal:noise Xevo TQ 0 Time Time

16 Ultra Trace Analysis What are we trying to do? Whole product Representative sample Ultra trace detail

17 Ultra Trace Analysis What is in a sample? Grape Marjoram Avocado Ginger

18 Xevo TQ MS Technology Ion Optics Mass spectrometer ScanWave collision cell- Operated in travelling wave mode

19 Full scan - MS2 Transfer Transfer Transfer

20 MS/MS mode : MRM

21 Dual Scan-MRM (DS-MRM) Rapid switch between MRM and MS2 full scan acquisition modes. 3 ms

22 DS-MRM Experiment set-up Full scan function 200 ms ( m/z) MRM function

23 Impact of Sensitivity RADAR data for complex samples Original Sample x10 dilution x100 dilution Acquisitions allow levels of matrix to be monitored during MRM analysis

24 x 10.2 decrease x 2.5 decrease Impact of Sensitivity Diluting Away Matrix Effects Peak Area PFHxA x10-75% suppression Reducing ion suppression x Expected RT

25 Ultra Trace Analysis Matrix Effects High Matrix background Azinphos -ethyl Atrazine Low calculated recoveries Simetryn Poor peak shape Cyromazine DisQuE Ginger QC extract 0.01 mg/kg (10 ppb)

26 Ultra Trace Analysis Reduced Matrix Effects Reduced Matrix background Azinphos -ethyl -54% Atrazine -58% Reduced ion suppression Simetryn -47% Improved peak shape Cyromazine 10 x dilution of Ginger extract All peaks detected, recoveries good

27 Xevo TQ MS and Xevo TQ-S 6 Sources available ESCi combined ESI/APCI ASAP Atmospheric Pressure Solid Analysis Probe Nanoflow-ESI (nano ACQUITY) TRIZAIC Microfluidic UPLC Separation ESI Combined APCI/APPI APGC Atmospheric Pressure GC

28 ASAP Atmospheric pressure Solids Analysis Probe Direct sample analysis Fast (<1 minute) No sample prep No chromatography Solids and liquids Available for all Waters mass specs (newer generations)

29 ASAP How does it work The sample is applied to a glass melting point capillary and inserted into a heated stream of gas ( C) which vaporises the sample. The probe consists of two parts, an outer assembly and an inner probe which holds the melting point capillary securely in place. Licensed from M&M Mass Spec Consulting excusively to Waters Corporation

30 % % ASAP Determine different oil origin 4- Extra virgin olive oil (Sitia, Crete), 500 L/hr, C ASAP_02May08_07 55 (1.104) Cm (39:89) Oleic acid 1: TOF MS AP+ 3.37e5 Squalene Palmitic acid Diglycerides m/z Rapeseed oil, 500 L/hr, C ASAP_02May08_09 64 (1.283) Cm (49:90) : TOF MS AP+ 8.84e4 Oleic acid Linolenic acid Diglycerides m/z

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