Changing the Game in LC-MS/MS. New Tools for Unprecedented Performance in Residue Analysis. Dr. Thomas Glauner
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1 Changing the Game in LC-MS/MS New Tools for Unprecedented Performance in Residue Analysis Dr. Thomas Glauner EMEA LC/MS Food Segment Scientist Agilent Technologies Waldbronn
2 The New 6490 Triple Quadrupole LC/MS 6490 Technology Review ifunnel Curved Collision Cell Electronics Sensitivity Enhanced Resolution Data Review Sensitivity Data Pesticides and PPCPs in Water Software tools for QQQ applications 2
3 6490 The New High Sensitivity Triple Quadrupole Ionization and Ion Transfer Technology Agilent Jet Stream Ion Generation Hexabore capillary Dual ion funnel (DIF) technology Two stages for ion focusing and gas removal Improvements for wide m/z range transmission Low capacitance Collision Cell Hexapole field axial focusing curved collision cell Tapered cell structure for increased ion acceptance at entrance Reduced noise Improved Quad Drive Electronics Improved Quad DC frequency response Higher RF power capability Quad drive frequency increased to 1.4 MHz 3
4 Hexabore Atmospheric Sampling. SIX bores HALF as long 6 Bore Capillary Six bores, Half the restriction means 6 times the amount of atmospheric gas sampled AND 5 10X the number of ions sampled over wide mass range. But how do we handle all the extra gas molecules? Compare: Standard Capillary is 180mm 4
5 Agilent s Two Stage Ion Funnel Can Handle the Gas Load High Pressure Stage 1 Low Pressure Stage 2 Existing RF Ion Guide Stage Torr Stage Torr Stage 1 offset breaks up the high pressure gas exiting the Hexabore Capillary 5
6 How Does an Ion Funnel Work? RF Voltage focuses the ions to the center. RF Drive Unfocused Ions and Gas Enter Focused Ions Out DC Voltage accelerates the ions to the exit. DC Drive
7 Triple Quadrupole Instrument Configurations 6460 LC/MS (Skimmer Configuration) Cap RF Ion Q1 Coll Q3 Guide Cell Ion Detector Ion Detector Q LC/MS (ifunnel Configuration) Curved Collision cell HB Cap Dual Ion RF ion Q1 Funnels guide
8 Improved Ion Sampling Efficiencies Agilent Jet Stream positive ion Agilent Jet Stream negative ion 7x 7x 7x 5x 5x x 11x 10x 7x 10x m/z m/z
9 6490 with ifunnel vs 6460 in Positive Ion Mode 1 pg Reserpine (7X) 1 pg Alprazolam (6X) x x Time (min) Time (min) 9
10 6490 with ifunnel vs 6460 in Negative Ion Mode 1 pg Chloramphenicol (8X) 1 pg Acid red 4 (9X) x x Time (min) Time (min) 10
11 New 6490 Triple installation Spec: S/N > 10,000:1 so the 6490 should be able to detect 1 fg? 1 pg reserpine on-column S/N > 22,605:1
12 The Attogram Sensitivity for Reserpine 1 fg of reserpine injected on-column S/N is as predicted Time [min]
13 Trace Analysis of Pharmaceuticals: Overall Goals Instrumentation Evaluation 6490 for Direct Aqueous Injection Wastewater Analysis Drinking Water Analysis and the 1 ppt Detection Barrier Data generated by: E. Michael Thurman and Imma Ferrer Dept of Civil, Environmental, and Architectural Engineering Center for Environmental Mass Spectrometry (CEMS), University of Colorado, Boulder, CO, USA
14 Albuterol: 1 ng/l Direct Injection in Water 40 fg on column LOD 1 ng/l Albuterol: Bronchodilator OH HO H N C(CH 3 ) 3 HO 5 ng/l Albuterol
15 Dehydronifedipine: 40 fg on column from Water Sample LOD 1 ng/l Dehydronifedipine: Anti-anginal H 3C N CH 3 H 3CO OCH 3 O O NO 2 5 ng/l
16 High sensitivity achieved with combination of Jet Stream and ifunnel Technology Carbamazepine ng/l QqQ 6410 QqQ 6460 Jet Stream QqQ 6490 Ion Funnel Acetaminophen ppb 3 times 20 times Caffeine ppb 2 times 10 times Carbamazepine ppb 3 times 20 times Sulfadimethoxine ppb 3 times 20 times
17 Limits of Detection for 6490 with Direct Aqueous Injection of 40 µl water sample Compound On Column (fg) LOD in Water sample Compound On Column (fg) LOD in Water sample Acetaminophen ppt Albuterol 40 1 ppt Atenolol ppt Caffeine ppt Carbamazepine 40 1 ppt Cotinine ppt Dehydronifedipine 40 1 ppt Diltiazem ppt Diphenhydramine ppt Metoprolol ppt Sulfadimethoxine ppt Sulfathiazole ppt Trimethoprim ppt Diclofenac (Neg Ion) ppt Gemfibrosil ppt Naproxen 20, ppt Triclocarban ppt Triclosan ppt
18 Trace Analysis in Water using the 6490 Poster at ASMS
19 6490 Pesticide Analysis Calibration Plots Example Calibration Plots, ppt (6 levels, 3 replicates.) Mexacarbate (carbamate insecticide) Fenuron (phenylurea herbicide) 1 ppt SNR 326 R 2 = ppt SNR 50 R 2 = Secbumeton (triazine herbicide) Metolachlor (chloroacetanilide herbicide) 1 ppt SNR 32 R 2 = R 2 = ppt SNR 225 Low PPT to sub-ppt level detection of pesticides in water by on-line SPE-LCMS/MS 19
20 Ultra Trace Levels of Pesticides in Potable Water 11 Triazine herbicides analyzed at 50 parts per quadrillion level in water Atraton s/n: 819 s/n is calculated based upon peak height and 5*RMS noise 6490 Triple Quad with online enrichment Simazine s/n: 18 Ametryn s/n: 56 Simetryn s/n: 9 Propazine s/n: 15 Secbumeton s/n: 51 Terbuthylazine s/n: 33 Prometon s/n: 40 Prometryn s/n: 54 Atrazine s/n: 28 Terbutryn s/n: 59 20
21 Fast method setup using LC/MS Application Kits Add Application Kit to your LCMS Instrument: - pre-defined methods - Accurate mass databases and libraries for TOF and QTOF - Dynamic MRM databases for QQQ Use one of the following Application Kits: G6854AA -- Pesticide Personal Compound Database kit G3876AA PCDL Database & Library Forensics/Toxicology kit G1733AA -- Pesticides Dynamic MRM Database Kit G1734AA -- Forensic/Tox Dynamic MRM Database Kit 21
22 Fast review with new Compounds at a Glance Free configurable peak review window allows fast reviewing up to 100 compounds and samples at one time New MH Quant B organize by samples or compounds - overlay of qualifiers or ISTDs - normalize axis - flag for outliers 22
23 New 6490 LC Triple with ifunnel Technology Conclusion 1290 Infinity LC/6490 Triple : Clearly Better Together High Pressure High Speed High Sensitivity
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