Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in...

41
Innovation with Integrity Bruker Corporation

Transcript of Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in...

Page 1: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Innovation with Integrity

Bruker Corporation

Page 2: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

50 Years of Bruker History

1960 Bruker was founded in 1960 with NMR products

2006 Bruker BioSciences acquires Bruker Optics

2003 Merger of Bruker Daltonics and Bruker AXS into Bruker BioSciences (BRKR)

1974 First Bruker FT-IR developed internally

1980 Bruker acquires/develops mass spec business, later called Bruker Daltonics

1997 Bruker acquires analytical X-ray business from Siemens, called Bruker AXS

2001 Bruker AXS IPO

2000 Bruker Daltonics IPO

2007 Bruker BioSciences (BRKR) and separate private Bruker BioSpin (NMR/MRI)

2008 Merger of Bruker BioSciences and Bruker BioSpin into Bruker Corporation (BRKR)

2010 Acquisition of GC, GC-QQQ and ICP-MS Technologies

Page 3: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Global Company with Diversified Markets

Other R&D and Production Sites

Sales, Applications & Service Offices

US and European (DE, CH, FR, NL) Major R&D and Production Sites

Headquarters

3

• Over 5,500 Employees in over 90 Countries around the world

Page 4: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Bruker Corporation

• Bruker AXS –X-ray, optical emission spectroscopy, atomic force microscopy and stylus and optical metrology instrumentation

• Bruker BioSpin – Magnetic resonance spectroscopy and imaging (NMR, MRI, EPR)

• Bruker Daltonics - Mass spectrometry, gas chromatography and CBRN detection

• Bruker Optics – Optical Vibrational Spectroscopy (FT-IR , NIR & Raman)

Bruker Energy & Supercon Technologies (BEST)

• Super conducting magnets, high and low temperature wire development and manufacturing

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Page 5: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Innovation with Integrity

Copyright © 2011 Bruker Corporation. All rights reserved. www.bruker.com

Page 6: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Impact HD: High-Definition bench-top UHR-QTOF

Highlighting the new Impact HD QToF for Screening & Identification of Unknowns and Sample Data Review

Sandy Yates, Bruker

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Page 7: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Outline

• Impact HD Q-ToF for Screening

• Identification of Unknowns

• Sample Data Review

2

Page 8: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Bruker’s New impact HD Bench-top QTOF

• High Definition: 5 orders of magnitude dynamic range at UHPLC speed from 10-Bit digitizer technology - definitive trace analysis from complex, high-background matrices

• Full mass resolution (40,000 @ m/z 1222) at full sensitivity

• Instant Expertise: Intelligent dynamically optimizing MS/MS for easier tandem MS work

3

Introducing High-Definition, Instant Expertise™ and in Ultra-High performance LC-MS-MS bench-top QTOF

Page 9: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

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How does Impact HD achieve the performance?- Dual Ion Funnel Source ( Introduced 2005 )- Increased sensitivity, reduced method tuning

Page 10: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

2121.9211

2122.9241

2123.9254

140107‐NI5155ave_high_gesaettigt_Wdh000001.d: +MS, 1.7‐51.2s #1‐49

2121.9446

2122.9407

2123.9417

121213_U1084A_ave_high_000001.d: +MS, 3.2‐19.2s #3‐19

2120 2122 2124 2126 2128 m/z0

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4

6

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6x10Intens.

2121.93321+

2122.93641+

2123.93941+

2124.94221+

C₄₂H₁₉F₇₂N₃O₆P₃, M, 2121.9332

0

500

1000

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Intens.

2120 2122 2124 2126 2128 m/z

theoretical10-bit ADC

8-bit ADC

Impact HD: More Dynamic Range = Accurate Quantitation

• 3-4 x higher dynamic range from 10-bit ADC technology

• Provides highest sampling speeds and maintains high resolution

2x time higher concentration:12C peak still not in saturation

12C peak in saturation13C/ 12C peak ratio incorrect

5

Direct benefit for quantitation and

identification

Page 11: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

8.32 min

9.47 min

6.22 min

5.64 min9.54 min

9.00 min10.90 min

11.67 min

10.95 min

9.64 min

9.28 min9.28 min 11.62 min

9.83 min12.89 min11.60 min11.74 min11.72 min 12.73 min10.82 min 14.22 min12.85 min13.11 min13.20 min13.31 min13.11 min13.20 min13.31 min 14.20 min10.92 min

7.86 min 9.98 min 11.09 min

9.07 min

7.06 min5.50 min 6.25 min

5.26 min

9.19 min5.17 min4.35 min 11.13 min

9.35 min 10.83 min11.25 min

11.33 min10.56 min9.83 min

9.69 min3.81 min 12.80 min4.76 min 9.64 min 11.42 min

4.16 min 9.48 min12.10 min6.10 min 10.13 min1.44 min

10.10 min8.77 min12.63 min10.85 min10.03 min 12.51 min11.90 min

13.81 min8.94 min3.36 min 10.49 min 11.25 min 13.01 min

60_Pesticides Mix 2.5 ppm F_BC1_04_6084.d

7.87 min 11.12 min9.07 min5.25 min5.17 min 11.23 min9.53 min9.22 min6.20 min 10.83 min 12.81 min5.62 min 9.02 min9.35 min 12.88 min10.55 min10.90 min11.33 min 12.50 min9.83 min

3.80 min 9.63 min9.48 min11.60 min11.62 min9.28 min

9.82 min 11.72 min10.02 min 14.20 min12.85 min13.20 min13.31 min13.31 min13.20 min12.46 min 14.21 min13.10 min13.10 min10.85 min10.95 min

9.48 min5.50 min 11.10 min8.32 min 9.98 min7.07 min6.25 min 11.67 min 12.63 min4.35 min10.95 min

9.68 min 12.08 min4.15 min 4.77 min 9.63 min 11.45 min

12.73 min6.10 min 10.85 min10.13 min9.28 min 11.73 min1.44 min 8.77 min 10.10 min11.92 min 13.01 min 13.80 min3.35 min 8.93 min 10.52 min 11.28 min

60_Pesticides Mix 2.5 ppm_BC1_01_5945.d0.0

0.2

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1.0

7x10Intens.

0.0

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2 4 6 8 10 12 Time [min]

Other 8 bit system

Impact HD with 10-bit digitizer

Screening:more dynamic range - more confidence

60 pesticides at 2.5 ppm conc.

Enhanced sensitivity through broad mass transfer

Gain in dynamic range

Page 12: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

314.0731 m/z

0285 290 295 300 305 310 315 m/z

289.1219 m/z

0.00

0.02

0.04

0.06

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Intens.

[%]

288.4 288.6 288.8 289.0 289.2 289.4 289.6 289.8m/z

Intra-Scan Dynamic Range

7

9.2 9.4 9.6 9.8 10.0Time [min]EIC 289.1215±0.005, 8.74 - 10.74 min, +All MS FullScan, Myclobutanil, C 15 H 17 Cl 1 N 4 (9.7)EIC 314.0723±0.005, 8.89 - 10.89 min, +All MS FullScan, Triazophos, C 12 H 16 N 3 O 3 P 1 S 1 (9.9)

Coeluent LC peaks from a complex pesticide mix in Matrix

Page 13: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

195.087608

219.106753

+MS, 1.0min #55

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60 80 100 120 140 160 180 200 220 m/z

61.039693

+MS, 1.0min #55

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60.0 60.5 61.0 61.5 62.0 62.5 m/z

Caffeine 0.6ppmI = 9,230,400 counts

Urea 0.8 ppm I = 52 counts

>5 orders of magnitude dynamic range @ 1 Hz speed LC timescale

10-bit = Dynamic range at real LC speedMuch higher dynamic range in concentration reachable

Innovation with Integrity 8

1.7 x 105

Page 14: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

High-Definition Quantitation with hrEICover a large dynamic range

9

0,000E+0

1,000E+4

2,000E+4

3,000E+4

4,000E+4

0 500 1000 1500 2000 2500 3000

cou

nts

ppb

Calibration curve

High-Definition 10 bit

8 bit

Gain in dynamic range with High-Definition 10-bit Digitizer

More than 4 orders of magnitude: 100 ppt up to 2.5 ppm

y= 1995+x*13,513

R2=0.9996

Page 15: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

High-Definition Quantitation with hrEIC

10

0,000E+0

02E+4

04E+4

06E+4

08E+4

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

cou

nts

ppt

calibration curve

High-Definition 10 bit

8 bit

9.18 min

60_Pesticides Mix 100ppt F_BA4_05_6007.d: Imazalil, 297.0556±0.001, C 14 H 14 Cl 2 N 2 O 1, 9.3min

0

100

200

300

400

Intens.

8.4 8.6 8.8 9.0 9.2 9.4 9.6 9.8 10.0 Time [min]

Imazalil at 100ppt measured with Impact HDhrEIC @ 1 mDa width

EIC: S/N > 3 @ 100 ppt

R2=0.9996

Page 16: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

October 23, 2013 11

Data Dependant Tandem MS(AutoMS)

Now made easy with Instant ExpertiseTM

Page 17: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Instant Expertise: Optimal quant and ID results in One acquisition

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Challenge: Classical Auto MS/MS use basically the same pre-set conditions for fragmentation, independent of the peptide amount and chromatographic resolution - dynamic range and MS/MS quality is compromised

Solution: Instant Expertise Software with new autoMSMS strategies• IDAS™ (Intensity Dependent Acquisition Speed) • RT2™ (Real-Time Re-Think)

One acquisition method for all concentration levels

Higher yield of excellent MS/MS spectra => higher ID rates

Accuracy for quantitation

Page 18: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

BA

Instant Expertise™ RT2 : Real Time Re-Think

Innovation with Integrity 13

RealTime Re-Think managements of the Dynamic exclusion. The basic exclusion time is fixed to slightly longer than the base width of the chromatographic peak. Robust method to avoid unnecessary AutoMSMS events (never on falling peak flank)

B: The MS/MS is triggered a first time near the peak base => the precursor is reconsidered for fragmentation

A: The MS/MS is triggered near the peak maximum => the precursor is not fragmented again

Higher yield of good MS/MS => higher ID rates

Page 19: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

0.00

0.50

1.00

1.50

2.00

1 2 3 4

MS MS MS MS

30 MS/MS 29 MS/MS 16 MS/MS 21 MS/MS

Auto

MSM

S c

ycle

tim

e [s

]

AutoMS/MS cycles18 19

Always optimal results independent from sample amount or complexity

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IDAS (Intensity Dependent Acquisition Speed)

Number of MS/MS precursor ions automatically adjusted to precursor signal intensity

# of MS/MS spectra within 2.5 sec

Page 20: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

October 23, 2013 15

Identifcations of unknowns

Page 21: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Mass accuracy alone is insufficient for a unique compound identification or confirmation!

0

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90

100

50 100 150 200 250 300 350 400 450 500

5 ppm2 ppm

0.5 ppm

1 ppm

0.1 ppm

0.05 ppm

Majority of compounds to be analyzed

maximum of C200H400N50O50S5P5F5Cl5Br5I5, even electron configuration, nitrogen rule

Page 22: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

… However, even with very high mass accuracy (<1 ppm) many chemically possible formulae are obtained in higher mass regions. In automatic routines an additional orthogonal filter therefore needs to be applied in order to reduce the number of potential elemental compositions. …

Page 23: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

simulated spectrum of Reserpine [M+H]+ C33H41N2O9

609.280657

610.283932

611.286709

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500

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2000

2500

609.0 609.5 610.0 610.5 611.0 611.5 612.0 612.5 m/z

612.289405

2

1

2 Mass positions and distances of all isotope signals

2

1 Intensity of all isotope signals

13C – 12C : 1.0033548 Da

2H – 1H : 1.00627675 Da

15N – 14N : 0.997035 Da

34S – 32S : 1.9957959 Da

SigmaFit: used in SmartFormula(3D)

– Compares Isotope Pattern: measured versus theoretical

Page 24: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

19

Unambiguous Molecular Formula Determination with the new SmartFormula3D

Molecular Confidence Solution- Identification of unknowns- Verification of knowns (accurate mass & Isotopes )

Page 25: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Confirmation of sum formulae with instant accurate mass and isotopic fidelity

Perfect fit of isotopic ratios and spacing

SmartFormula™ does confirm the identification in spite of matrix background signals.

N

N

N

Cl Cl

284.0720

285.2057

286.0693

287.0727 288.0673

+MS, 10.80‐10.95min #633‐642, found: Penconazole, 283.0643, [[M+H]+: 284.0716])

284.0716

285.0745

286.0688

287.0716 288.0662

Penconazole, 283.0643, err[mDa]: 0.45, mSigma: 8.0)

284.0 284.5 285.0 285.5 286.0 286.5 287.0 287.5 288.0

Penconazole (C13H15Cl2N3)

Measured specturm

Theoretical spectrum

20

Page 26: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

10ppb Imazalil - 0.5 ppm mass accuracy - true isotopic pattern

Highest Confidence in Identification and Confirmation of Sum Formula due to Spectral Fidelity and SmartFormula™

297.0557

298.0583

299.0529

300.0560 301.0503

25.

Measured

297.0556

298.0587

299.0528

300.0558 301.0504

25. Theoretical0

Intens.[%]

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40

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100

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297 298 299 300 301 m/z

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80

100

• All 5 isotopes match• Unambiguous identification of

C14H15Cl2N2O, Imazalil with SmartFormula™

A+2= 65.4%

A+2= 65.3%

A+1= 16.1%

A+1= 16.3%

A+3= 10.4%

A+3= 9.8%

A+4= 11.1%

A+4= 9.9%

Page 27: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Summary: Impact HD Bench-top QTOF

• High Definition: 5 orders of magnitude dynamic range at UHPLC speed from 10-Bit digitizer technology - definitive trace analysis from complex, high-background matrices

• mSigma (Isotope Pattern Comparision), ID unknowns, conformation of known compounds

• Full mass resolution (40,000 @ m/z 1222) at full sensitivity

• Instant Expertise: Intelligent dynamically optimizing MS/MS for easier tandem MS work

22

Page 28: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Targeted Screening

Page 29: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Triple Quad and/or QToF:

TargetedQuantitative

Analysis

Unknown(Qualitative)ScreeningLC-Triple Quad LC-QTOF

Increasing confidence in IDIncreasing throughput in routine quant

Applied Markets Product Positioning Continuum

Food Testing:• High sensitivity, routine quant of

pesticides, veterinary drugs or toxin residues

Environmental Testing:• High sensitivity, routine quant of

pesticides, veterinary drugs or toxin residues

Clinical Research:• Targeted quant of drugs or

metabolites

Food Testing:• High sensitivity, routine quant of

pesticides, veterinary drugs or toxin residues

Environmental Testing:• High sensitivity, routine quant of

pesticides, veterinary drugs or toxin residues

Clinical Research:• Targeted quant of drugs or

metabolites

Food Testing:• Rapid screening of pesticides,

veterinary drugs or toxin residues

Toxicology (forensic and clinical):• Detailed screening and confirmation

of drugs of abuse or poisons

Environmental Testing:• Detailed discovery and screening of

pesticides, pharmaceuticals and personal care products (PPCP’s)

Food Testing:• Rapid screening of pesticides,

veterinary drugs or toxin residues

Toxicology (forensic and clinical):• Detailed screening and confirmation

of drugs of abuse or poisons

Environmental Testing:• Detailed discovery and screening of

pesticides, pharmaceuticals and personal care products (PPCP’s)

Page 30: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Copyright 2013 Bruker Corporation.  All Rights Reserved.  25Copyright 2013 Bruker Corporation.  All Rights Reserved.  25

Atrazine

Report

Processing:

TargetAnalysis

IdentificationConfirmation

Sample

Pesticidesfood, feed, waterenivronmental

Bruker‘s Target Screening  Solution

LC-QTOF-MS:

UHPLC + impactHigh sensitivityhigh resolution

accurate mass datatrue isotope pattern

Page 31: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Copyright 2013 Bruker Corporation.  All Rights Reserved.  26Copyright 2013 Bruker Corporation.  All Rights Reserved.  26

UHPLC‐TOF/MS analysis (sample 1 ... sample n)

Find all components:Get hrXIC of every compound, detect peaks and integrate

Screen: Check compounds against database, potential residues

Confirm compound:Match and score retention time, mass, isotopes, fragments, etc. Exceeds MRL?

Screening Report

Generic Extraction

High Resolution Full Scan Analysis For Rapid Screening

Page 32: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Copyright 2013 Bruker Corporation.  All Rights Reserved.  27Copyright 2013 Bruker Corporation.  All Rights Reserved.  27

Screener High Quality DatabaseMultiple dimensions of confirmation, required for larger databases due to false positives 

• Not just a “list of accurate mass compounds”

• Retention times for the matched UHPLC method• In-source Fragment ions• Isotopic pattern• Adduct information• Isomer information

• MS/MS Qualifier Ions for extra confirmation (broadband CID)

Enabling fast and reliable identification of selected compounds at ppb levels in a complex sample matrix, with very low false positive rates.

Page 33: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Copyright 2013 Bruker Corporation.  All Rights Reserved.  28Copyright 2013 Bruker Corporation.  All Rights Reserved.  28

Automated Data Processing – Target Analysis

• Visual review of the residues screened & scored against the database information • Retention Times, Accurate Mass, Isotopic Pattern (mSigma)• Broadband MS/MS qualifier ions (and their intensity ratios) for additional confirmation

• Enables fast and reliable identification of residues at ppb levels, with very low false positive rates even in complex matrices

Level of confidence

Page 34: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

AvermectinB1a (Abamectin) (NH4)Pesticides 10ppb CE8eV _BB1_02_29.d: AvermectinB1a (Abamectin) (NH4),

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13.4 13.6 13.8 14.0 Time [min]

6Oxamyl Fragm 72Pesticides 10ppb CE8eV _BB1_02_29.d: Oxamyl Fragm 72, 72.0444±0.003, C

0

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3.4 3.6 3.8 4.0 4.2Time [min]

Multi-Target Screening - 60 pesticides at 10ppb

Cyprodinil

MetalaxylTebufenozide Fragm 297

Methoxyfenozide Fragm 313 EthionCarbendazimAcetamipridThiabendazole

PenconazoleLinuron ProchlorazTebuconazoleMonocrotophos Dimethomorph Peak 2 ProfenophosPropargite Fragm 231Kresoxim-methyl

Methoxyfenozide Difenoconazole Peak 1Difenoconazole Peak 2Dimethoate Fragm 199 Cyhalothrin. lambda- (NH4)Dimethomorph Peak 1Monocrotophos Fragm 193 Fludioxonil (NH4) Indoxacarb (Na)FenhexamidTolyfluanid Ethion Fragm 199Phosmet Fragm 160Kresoxim-methyl Fragm 206Azoxystrobin Fragm 372Azinphos-methyl (Guthion) Prochloraz Fragm 308Tolyfluanid Fragm 238Azinphos-methyl Fragm 132Carbaryl Fragm 145 EPNTolyfluanid (NH4)Carbendazim Fragm 160Monocrotophos Fragm 98Oxamyl Fragm 90 PendimethalinQuinoxyphenSpinosad A (Spinosyn A) Fragm 5446 Pendimethalin Fragm 212Oxamyl Fragm 72 Cypermethrin III (NH4)Azinphos-methyl (Guthion) (Na)Monocrotophos Fragm 127 Chlorpyriphos-methylChlorantraniliprole (Na)Methomyl Fragm 106Oxamyl (NH4)

Pyriproxyfen

Trif loxystrobinTriazophos

DiazinonAzoxystrobinEtofenprox (NH4)

PirimicarbPyraclostrobin

Pyrimethanil Propargite (NH4)Thiacloprid CarbofuranImazalil

Spinosad A (Spinosyn A)Phosmet

Dimethoate IndoxacarbMyclobutanilOmethoateImidacloprid Boscalid Chlorpyriphos Bifenthrin (NH4)TebufenozideChlorantraniliproleCarbaryl Spinosad DMethomyl Fragm 88 Aldicarb Fragm 116 Chlorpropham Fragm 172

4 6 8 10 12 14 Time [min]0

1

2

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4

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4x10Intens.

• Single MS method for all analytes• Uncompromised mass range and sensitivity for small molecule

screening, e.g. 50-1000

m/z = 72.0444Δm/z = 0.5 ppm

m/z = 890.5267Δm/z = 1.6 ppm

XIC

29

Page 35: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Copyright 2013 Bruker Corporation.  All Rights Reserved.  30Copyright 2013 Bruker Corporation.  All Rights Reserved.  30

Detection & Identification‐ Full Scan MS, Orange, Spiked 10 ppb, 60 compounds

Triadimenol I Fragm 70

Triadimenol II Fragm 70

Oxamyl Fragm 72

Butocarboxim Fragm 75

Amitrole

Methomyl Fragm 88

Aldicarb Fragm 89

Oxamyl Fragm 90

Monocrotophos Fragm 98Methomyl Fragm 106

Aldicarb Fragm 116

Monocrotophos Fragm 127

Azinphos-methyl Fragm 132Tolyfluanid Fragm 137

Methamidophos

Carbaryl Fragm 145

Phosmet Fragm 160

Azinphos-methyl Fragm 160Carbendazim Fragm 160

Methomyl

Carbofuran Fragm 165

Chlorpropham Fragm 172

Omethoate Fragm 183 Butocarboxim

Carbendazim

Monocrotophos Fragm 193Dimethoate Fragm 199 Ethion Fragm 199

Pyrimethanil

Thiabendazole

Carbaryl

Kresoxim-methyl Fragm 206

Aldicarb (NH4)

Pendimethalin Fragm 212

Omethoate

ChlorprophamOxamyl Carbaryl (NH4)

Carbofuran

Acetamiprid

Monocrotophos

Cyprodinil

Dimethoate

Propargite Fragm 231

Oxamyl (NH4) Tolyfluanid Fragm 238

Pirimicarb

Monocrotophos (NH4)

Linuron

Fludioxonil

Thiacloprid

Imidacloprid

Fludioxonil (NH4)

Metalaxyl

Pendimethalin

Penconazole

Myclobutanil

Triadimenol II

ImazalilTebufenozide Fragm 297

Fenhexamid

Diazinon

Quinoxyphen

Tebuconazole

Prochloraz Fragm 308

Triazophos

Kresoxim-methylMethoxyfenozide Fragm 313

Phosmet

Azinphos-methyl (Guthion)Triadimenol II (Na)

Chlorpyriphos-methyl

Pyriproxyfen

EPN

Kresoxim-methyl (NH4)Phosmet (NH4)

Boscalid

Tolyfluanid

Chlorpyriphos

Propargite

Tebufenozide Etofenprox Fragm 359Tolyfluanid (NH4)

Propargite (NH4)

Methoxyfenozide

Profenophos

Azoxystrobin Fragm 372

Prochloraz

Ethion

Pyraclostrobin

Dimethomorph Peak 2Dimethomorph Peak 1

Etofenprox (NH4)

Azoxystrobin

Difenoconazole Peak 1Difenoconazole Peak 2

Trifloxystrobin

Cypermethrin II

Cypermethrin II (NH4)Cypermethrin III (NH4)Cypermethrin II (Na)Cypermethrin III (Na)

Bifenthrin (NH4)Cyhalothrin. lambda- (NH4)

Cyhalothrin. lambda- (Na)Chlorantraniliprole

Indoxacarb

Spinosad A (Spinosyn A) Fragm 544Indoxacarb (Na)

Spinosad D (Fragm 558)Spinosyn B or K (last of 3-4 peaks)

Spinosad A (Spinosyn A)

Spinosad D AvermectinB1a (Abamectin) (NH4)

AvermectinB1a (Abamectin) (Na)

2 4 6 8 10 12 14 Time [min]0

2

4

6

8

4x10Intens.

60615 24

1 9 267 141028

15 38 732

34

42392111 30 563 252216 19 944929 32 6727 994 576 33

311812 7720 1028 703513 48 512317 5236 1007458 6246 6564

76 9875 8059 68544140 63 8996

906943 50 71 9710366 11472101

55 9345 81 95785347

11544 8485

88106107109108110 11310410537 8682 87 917983 92 111112

2 4 6 8 10 12 14 Time [min]0.0

0.5

1.0

1.5

2.0

2.56x10

Intens.

BPC

hrXICsfor target compounds

100.0755

373.1302

622.0290 767.2326

41. +MS, 8.83-9.05min #523-536, found: Phosmet (C 11 H 12 N 1 O 4 P 1 S 2 , 316.9945, [ [M+H]+: 318.0018])

318.0018

41. Phosmet(C��H��N�O�P�S�, 316.9945, err[mDa]: -0.15, mSigma: 9.1)0.00

0.25

0.50

0.75

1.00

1.25

6x10Intens.

0

2000

4000

6000

8000

100 200 300 400 500 600 700 800 900 m/z

phosmet,experimental,full scan

theoretical

317.0917

318.0020

319.0046319.9987

321.2063

41. +MS, 8.83-9.05min #523-536, found: Phosmet (C 11 H 12 N 1 O 4 P 1 S 2 , 316.9945, [ [M+H]+: 318.0018])

318.0018

319.0046 319.9991

41. Phosmet(C��H��N�O�P�S�, 316.9945, err[mDa]: -0.15, mSigma: 9.1)0

2000

4000

6000

8000

Intens.

0

2000

4000

6000

8000

317.0 317.5 318.0 318.5 319.0 319.5 320.0 320.5 321.0 m/z

ID by mass accuracy & isotope pattern

“hrXIC”= High‐resolution extracted ion chromatogram of the mass +/‐ 2mDa selectivity for detection

Page 36: Innovation with Integrity · 2018. 12. 4. · 50 Years of Bruker History 1960 Bruker was founded in 1960 with NMR products 2006 Bruker BioSciences acquires Bruker Optics 2003 Merger

Summary: Impact HD Bench-top QTOF

• High Definition: 5 orders of magnitude dynamic range at UHPLC speed from 10-Bit digitizer technology - definitive trace analysis from complex, high-background matrices

• mSigma (Isotope Pattern Comparision), ID unknowns, conformation of known compounds

• Targeted Screening, Quantification

• Full mass resolution (40,000 @ m/z 1222) at full sensitivity

• Instant Expertise: Intelligent dynamically optimizing MS/MS for easier tandem MS work

31

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© Copyright Bruker Corporation. All rights reserved.

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Sample Analysis:Impact HD Bench‐Top QTOF

33

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LC Method, (for reference only)HPLC system: Dionex RSLCColumn: Phenomenex Gemini 150x2 mm, 3 µmColumn Temp: 30CMobile Phase: 

MP‐A : 0.1% AcOH in H2OMP‐B : 0.1% AcOH in ACN

Injection Volume: 5 µLGradient:

LC Conditions

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Copyright 2013 Bruker Corporation.  All Rights Reserved.  35Copyright 2013 Bruker Corporation.  All Rights Reserved.  35

SmartFormulaMass error:  1.9ppmmSigma 4.2

EIC: 353.232 (2mDa)

Cayman ChemStandards

Concentration:1ppm

Initial Results: Cayman Chem: Standards

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© Copyright Bruker Corporation. All rights reserved.