Triple Quadrupole GC-MS/MS Re-imagined: Increased Simplicity and Productivity

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Information about Triple Quadrupole GC-MS/MS Re-imagined: Increased Simplicity and...
Technology

Published on March 10, 2014

Author: Chrom_Solutions

Source: slideshare.net

Description

Key Learning Objectives:

• Identify emerging triple quadrupole GC-MS/MS technology designed to address increasing regulatory demands and requirements
• Explore potential time savings in sample prep, method development/transition, and data analysis
• Demonstrate how to optimize the GC-MS/MS workflow from sample prep to sample analysis to automated data analysis

Overview:

Regulatory lab requirements continue to drive detection limits lower with an ever increasing list of compounds to analyze. These requirements also demand greater precision at these lower limits. Triple quadrupole GC-MS/MS is a viable option for enhanced analysis and increased productivity with an emphasis on simplicity. We discuss emerging trends and technologies designed to ensure that laboratories are well-equipped to address these increased demands with minimal investment in training and method development. Find out how you can adopt triple quadrupole GC-MS/MS technology in your laboratory using existing methods and source parameters in most instances while requiring less sample prep and enjoying the benefits of automated data analysis for increased simplicity and productivity.

For more information: www.thermoscientific.com/tsq8000

1 The world leader in serving science Increased Simplicity and Productivity Triple Quadrupole GC-MS/MS Re-imagined

2 Tough challenges faced in the laboratory • High sample loads/short deadlines • Keeping sample analysis costs down with more and more challenging LODs and matrices • Integrating and maintaining new methods and technologies into production workflows to remain competitive

3 What„s required... • Realization of the productivity advantages of high performance GC- MS/MS • Minimizing the impact of adoption and implementation to current laboratory operations

4 Triple Quadrupole GC-MS/MS is an essential part of a cost- effective, high productivity analytical method in today’s laboratory

5 Many laboratories are already investing in and exploring GC- MS/MS as a tool to obtain a competitive edge in their analyses

6 GC-MS/MS – What‟s so special? • Low detection limits • Reduced sample preparation • Consolidated analytical methods • Faster, automated data processing ...it is a high selectivity technique...

7 Selectivity in a method McLafferty circa. 1980

8 Method performance requirement • Target compounds • Matrices • Sensitivity Method performance requirement

9 First sample prep.. Step1–extraction Step2-cleanup(1st) Step3-cleanup(2nd) Method performance requirement

10 ...then instrument detection... Step1–extraction Step2-cleanup(1st) Step3-cleanup(2nd) Step4-GC-MSdetection(singlequadSIM) Total method selectivity Method performance requirement

11 Analytical Benefits for Single Quadrupole GC-MS • Robust • Run more samples between cleaning • Sensitive Precision • Accurate and reproducible results at the lowest levels • Unknown Analysis • Full scan for unknown library searches • Alternating full scan/SIM for unknowns and low level analysis • Flexibility • Switch quickly between dedicated EI and CI sources • Easy to Use and Maintain

12 Full Scan/SIM Methodology for Drinking Water

14 Challenging Samples for Single Quadrupole GC-MS • Matrix Challenges • Concentration challenges • Difficult to prove contamination Gamma BHC Methiocarb Mevinphos

15 ...what about GC-MS/MS?... Step1–extraction Step2-cleanup(1st) Step3-cleanup(2nd) Total method selectivity Step4-GC-MS/MSdetection(TriplequadSRM) Method performance requirement

16 Use GC-MS/MS to reduce clean-up... Step1–extraction Total method selectivity Step2-GC-MS/MSdetection(TriplequadSRM) Method performance requirement

17 Use GC-MS/MS to consolidate methods... Step1–extraction Total method selectivity Step2-GC-MS/MSdetection(TriplequadSRM) Method 1 performance requirement Method 2 performance requirement Method 3 performance requirement

18 Use GC-MS/MS to consolidate methods... Step1–extraction Total method selectivity Step2-GC-MS/MSdetection(TriplequadSRM) Consolidated multi-residue method

19 What will GC-MS/MS do for my lab? High selectivity • Possibility the reduce selectivity in sample preparation • Reduced sample prep steps creates a more generic sample prep method – more compounds & matrices • Consolidated GC-MS methods due to high performance – buffer against requirements • Compressed chromatography possible • Easy peak evaluation – auto- integrators

20 Step 1: Ions are produced in the source

21 Step 2: Ions are focused in the s-shaped prefilter

22 Step 2: Ions focused by prefilter, removing neutrals

23 Step 3: Ions are isolated by molecular weight in Q1

24 Step 3: Ions are isolated by molecular weight in Q1

25 Step 4: Ions further fragmented in collision cell (With same mass as analyte)

26 Step 4: Ions further fragmented in collision cell

27 Step 5: Unique ions to analytes chosen in Q3

28 Only unique fragments to analyte detected Step 5: Unique ions to analytes chosen in Q3

29 AutoSRM Overview 1) Precursor ion selection 2) Product ion selection 3) Collision energy optimization SRMCreationWorkflow

30 Step 1 – Pick Your Precursor Ions

31 Step 1 – Pick Your Precursor Ions

32 Step 1 – Pick Your Precursor Ions

33 Step 2 – Pick Your Product Ions

34 Step 2 – Pick Your Product Ions

35 Step 3 – Optimize Your Transitions

36 Step 3 – Optimize Your Transitions

37 Export from AutoSRM to Instrument Method

38 Timed-SRM Method Overview Acquisition Windows centered around retention time and Window

39 Timed-SRM Method Overview Acquisition windows allowed to overlap

40 Timed-SRM Advantages Segmented SRM Timed SRM

41 Timed-SRM Advantages Acquisition Windows Segmented SRM Timed SRM

42 Timed-SRM Advantages • Removes wasted dwell time • Allow higher overall dwell times • Leads to higher sensitivity Wasted Dwell Time

43 Timed-SRM Advantages • Peaks centered in acquisition window • No peak elutes near acquisition break • Allows for retention time shift (e.g. due to heavy matrix)

44 Instrument Parameters

45 Timed-SRM from Thermo Scientific TSQ 8000 GC-MS Screenshot of a section of the analytical run showing the “acquisition map” automatically created by the TSQ™ 8000 System using t-SRM.

46 Calibration Curves • All calibration curves correlation coefficients greater than 0.99 • Example calibration curve for Cyfluthrin, R2 = 0.9996

47 Transitions for Pesticides from PAR ver 2 • SRM peaks at 4 ppb from Terbacil (left, 161.1 > 88.0, CE 15 V) and Alachlor(right, 188.1 > 130.1, CE 25 V) • SRM peaks at 4 ppb from Tolylfluanid (left, 238.1 > 137.1, CE 15 V) and Pyridaben (right, 309.1 > 147.1, CE 15 V)

48 The world leader in serving science A Second Level of Selectivity Structure and Mass Defect

49 Thermo Scientific TSQ Quantum XLS Ultra – HyperQuad™ Technology Inside  Patented HyperQuad technology meets with GC/MS for the first time to create highest performing GC Triple on the market  6 mm hyperbolic precision quads allow excellent ion transmission at standard resolution as well as opportunity to use enhanced mass resolution to 0.1 Da peak width  Effective pre-cursor ion filtering with strongly reduced matrix interference  Improved signal/noise & quantitative precision

50 U-SRM: Two Modes of Selectivity •Ultra selective-Single Reaction Monitoring (U-SRM) •Offers a unique opportunity to increase selectivity using triple quadrupole. •Combination •Increased Q1 mass resolution •MS/MS Structural based selectivity •For use when standard SRM does not provide enough selectivity m/z Increased mass resolution Structural selectivity (MS/MS)

51 Precursor Ion Selection Q1 (Standard SRM mode) •At standard mass resolution precursor selection •Q1 = 0.7 Da FWHM •Higher probability that interfering species are transmitted to the collision cell with the target compound mass •These matrix interferents are often orders of magnitude higher than target compounds •If they are not completely discriminated against in by CID then the resulting product ion detection can have a higher background noise present Matrix components transmitted through Q1 during SRM Q1= 218.9 m/z (0.7 Da res.) Q1 Transmission Window Q1= 0.7Da 21921 7 22 1

52 219 Precursor Ion Selection Q1 (U-SRM mode) HyperQuad does not allow matrix through through Q1 during U-SRM • When operated in U-SRM mode, the TSQ Quantum XLS Ultra narrows the pre-cursor mass window to <0.2Da •This increased resolution allows the HyperQuad to discriminate against common matrix component masses for targets showing a large enough Δmass defect. •This allows for better collision cell performance and robustness as well as reducing chemical noise •Lindane carries a Δmass defect and can be isolated from matrix in this example Q1= 0.1Da 219217 221 Q1= 218.86 m/z (0.1 Da res.)

53 U-SRM: Effect of Increasing Q1 Resolution •Real life effect of the lindane example… •Lindane isomers in green tea •As Q1 resolution is increased into the ultra range signal/noise ratio increases dramatically IncreasingQ1resolution IncreasingSignal/Noise 0.1 Da 0.4 Da 0.7 Da

54 U-SRM in action • PCB 28 in industrial soil sample at ca.100fg (ASE extraction with no clean- up) • Continuum full scan spectrum shows background removed with HyperQuad at increased resolution contocpSCAN003 #1594-1597 RT: 13.68-13.69 AV: 4 SM: 7B NL: 4.04E7 T: + p EI Q1MS [200.000-300.000] 255.0 255.2 255.4 255.6 255.8 256.0 256.2 256.4 256.6 256.8 257.0 257.2 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance XLSULTRA_NPV_OCP00016_110329102653 3/29/2011 10:26:53 AM RT: 13.33 - 15.12 SM: 7G 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 15.0 Time (min) 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance RT: 13.69 14.54 14.4614.30 14.64 14.68 14.7214.40 14.16 14.7713.73 14.24 14.94 15.02 14.09 14.05 14.89 13.96 13.94 13.81 13.56 NL: 1.05E5 TIC F: + c EI SRM ms2 255.960 [185.965-185.975] MS XLSULTRA_NPV_OC P00016_110329102 653 SRM (Q1 0.7Da) 0.7 Da 256 m/z Q1 precursor selection 2,4,4'-Trichlorobiphenyl

55 U-SRM in action • PCB 28 in industrial soil sample at ca.100 fg (ASE extraction with no clean- up) • Continuum full scan spectrum shows background removed with HyperQuad at increased resolution. • Dramatically improved detection using U-SRM C:XCALIBUR...contocpSCAN004 4/14/2011 5:27:58 PM contocpSCAN004 #1469-1471 RT: 13.68-13.69 AV: 3 SM: 7B NL: 3.02E6 T: + p EI Q1MS [200.000-300.000] 255.0 255.2 255.4 255.6 255.8 256.0 256.2 256.4 256.6 256.8 257.0 257.2 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance contocpSCAN003 #1594-1597 RT: 13.68-13.69 AV: 4 SM: 7B NL: 4.04E7 T: + p EI Q1MS [200.000-300.000] 255.0 255.2 255.4 255.6 255.8 256.0 256.2 256.4 256.6 256.8 257.0 257.2 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance XLSULTRA_NPV_OCP00011_110329074139 3/29/2011 7:41:39 AM RT: 13.33 - 15.12 SM: 7G 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 15.0 Time (min) 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance RT: 13.69 NL: 3.21E3 TIC F: + c EI SRM ms2 255.960 [185.965-185.975] MS ICIS XLSULTRA_NPV_OCP 00011_110329074139 XLSULTRA_NPV_OCP00016_110329102653 3/29/2011 10:26:53 AM RT: 13.33 - 15.12 SM: 7G 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 15.0 Time (min) 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 RelativeAbundance RT: 13.69 14.54 14.4614.30 14.64 14.68 14.7214.40 14.16 14.7713.73 14.24 14.94 15.02 14.09 14.05 14.89 13.96 13.94 13.81 13.56 NL: 1.05E5 TIC F: + c EI SRM ms2 255.960 [185.965-185.975] MS XLSULTRA_NPV_OC P00016_110329102 653 U-SRM (Q1 0.1Da) Matrix interefent transmitted in standard mode (0.7Da) but rejected during U-SRM (0.1Da) precursor selection PCB 28 Precursor mass 2 55.96 m/z selected 0.1Da0.7Da SRM (Q1 0.7Da) 0.7 Da 0.1 Da

56 Environmental: Polychlorinated Biphenyls (PCBS) XLSULTRA_NPV_OCP00017_110329105955 3/29/2011 10:59:55 AM RT: 13.17 - 16.75 SM: 7G 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 Time (min) 0 50 100 0 50 100 0 50 100 0 50 100 RelativeAbundance 0 50 100 0 50 100 RT: 14.04 AA: 725579 SN: 97 RT: 14.35 AA: 37646 SN: 280 RT: 14.78 AA: 201199 SN: 229 RT: 15.03 AA: 140023 SN: 185 RT: 14.38 AA: 94563 SN: 88 RT: 16.03 AA: 24964 SN: 94 RT: 16.03 AA: 26376 SN: 160 NL: 1.01E5 TIC F: + c EI SRM ms2 255.960 [185.965-185.975] MS XLSULTRA_NPV_OCP00017_11 0329105955 NL: 1.53E5 TIC F: + c EI SRM ms2 257.960 [185.965-185.975] MS ICIS XLSULTRA_NPV_OCP00017_11 0329105955 NL: 1.37E4 TIC F: + c EI SRM ms2 289.920 [219.935-219.945] MS ICIS XLSULTRA_NPV_OCP00017_11 0329105955 NL: 7.06E4 TIC F: + c EI SRM ms2 291.920 [219.935-219.945] MS ICIS XLSULTRA_NPV_OCP00017_11 0329105955 NL: 1.01E4 TIC F: + c EI SRM ms2 323.880 [253.905-253.915] MS ICIS XLSULTRA_NPV_OCP00017_11 0329105955 NL: 1.42E4 TIC F: + c EI SRM ms2 325.880 [255.905-255.915] MS ICIS XLSULTRA_NPV_OCP00017_11 0329105955 XLSULTRA_NPV_OCP00011_110329074139 3/29/2011 7:41:39 AM RT: 13.17 - 16.75 SM: 7G 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 Time (min) 0 50 100 0 50 100 0 50 100 0 50 100 RelativeAbundance 0 50 100 0 50 100 RT: 13.69 AA: 5479 SN: 859 RT: 13.70 AA: 5485 SN: 862 RT: 14.37 AA: 4122 SN: 1454 RT: 14.36 AA: 1393 SN: 393 RT: 16.05 AA: 2033 SN: 352 RT: 16.04 AA: 3693 SN: 412 NL: 3.21E3 TIC F: + c EI SRM ms2 255.960 [185.965-185.975] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 NL: 2.87E3 TIC F: + c EI SRM ms2 257.960 [185.965-185.975] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 NL: 2.74E3 TIC F: + c EI SRM ms2 289.920 [219.935-219.945] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 NL: 1.02E3 TIC F: + c EI SRM ms2 291.920 [219.935-219.945] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 NL: 1.54E3 TIC F: + c EI SRM ms2 323.880 [253.905-253.915] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 NL: 2.53E3 TIC F: + c EI SRM ms2 325.880 [255.905-255.915] MS ICIS XLSULTRA_NPV_OCP00011_11 0329074139 Tri, Tetra, Penta PCBs 100 fg in Contaminated land (industrial soil) sample Standard SRM ( Q1=0.7 Da) TSQ Quantum XLS Ultra U-SRM ( Q1=0.1Da )

57 Environmental: Pesticides Endrin 1pg in contaminated land sample ran both in SRM (Q1 0.7 amu) and U-SRM (Q1 0.1 amu) U-SRM SRM C:Xcalibur...XLSULTRA_NPV_0104OCP048 4/2/20117:39:50 PM RT: 16.93 - 17.25 SM: 3G 16.95 17.00 17.05 17.10 17.15 17.20 Time (min) 0 20 40 60 80 100 0 20 40 60 80 100 0 20 40 60 80 100 0 20 40 60 80 100 NL: 1.68E5 m/z= 190.43-191.43 F: + c EI SRM ms2 262.910 [190.925-190.935, 192.925-192.935] MS XLSULTRA_NPV_0104OCP0 48 NL: 1.83E5 m/z= 192.43-193.43 F: + c EI SRM ms2 262.910 [190.925-190.935, 192.925-192.935] MS XLSULTRA_NPV_0104OCP0 48 NL: 1.25E4 m/z= 190.43-191.43 F: + c EI SRM ms2 262.910 [190.925-190.935, 192.925-192.935] MS ICIS xlsultra_npv_0104ocp031 NL: 1.86E4 m/z= 192.43-193.43 F: + c EI SRM ms2 262.910 [190.925-190.935, 192.925-192.935] MS ICIS xlsultra_npv_0104ocp031 XLSULTRA_NPV_OCP00015_110329095349 3/29/2011 9:53:49 AM RT: 15.48 - 17.07 SM: 7G 15.5 15.6 15.7 15.8 15.9 16.0 16.1 16.2 16.3 16.4 16.5 16.6 16.7 16.8 16.9 17.0 Time (min) 0 10 20 30 40 50 60 70 80 90 100 RelativeAbundance 0 10 20 30 40 50 60 70 80 90 100 RelativeAbundance RT: 16.56 AA: 28533 SN: 31RMS RT: 15.95 AA: 29627 SN: 31RMS 16.59 16.56 16.71 16.89 16.8416.65 16.7715.95 16.30 16.5016.38 16.23 16.43 16.0615.85 16.08 15.77 NL: 1.74E4 m/z= 175.47-176.47 F: + c EI SRM ms2 245.950 [175.965-175.975] MS ICIS XLSULTRA_NPV_OCP000 15_110329095349 NL: 7.78E3 m/z= 245.45-246.45 F: + c EI SRM ms2 317.940 [245.945-245.955] MS XLSULTRA_NPV_OCP000 15_110329095349 XLSULTRA_NPV_OCP00013_110329084745 3/29/2011 8:47:45 AM RT: 15.48 - 17.07 SM: 7G 15.5 15.6 15.7 15.8 15.9 16.0 16.1 16.2 16.3 16.4 16.5 16.6 16.7 16.8 16.9 17.0 Time (min) 0 10 20 30 40 50 60 70 80 90 100 RelativeAbundance 0 10 20 30 40 50 60 70 80 90 100 RelativeAbundance RT: 16.56 AA: 12784 SN: 708RMS RT: 15.95 AA: 7444 SN: 412RMS RT: 16.86 AA: 380 SN: 22RMS RT: 16.67 AA: 198 SN: 19RMS RT: 16.52 AA: 129 SN: 14RMS 16.56 15.95 16.53 16.6216.4116.11 16.2315.85 16.76 16.7916.3616.03 16.91 NL: 6.83E3 m/z= 175.47-176.47 F: + c EI SRM ms2 245.950 [175.965-175.975] MS ICIS XLSULTRA_NPV_OCP000 13_110329084745 NL: 1.16E3 m/z= 245.45-246.45 F: + c EI SRM ms2 317.940 [245.945-245.955] MS XLSULTRA_NPV_OCP000 13_110329084745 U-SRM SRM o,p-DDE & p,p-DDE 100fg in contaminated land sample ran both in SRM (Q1 0.7 amu) and U-SRM (Q1 0.1 amu)

58 • New technology • Sample through-put • Time savings • Lower detection limits • Triple Quadrupole GC-MS/MS provides selectivity with flexibility • Advanced Triple Quadrupole GC-MS/MS can deliver two modes of selectivity • Increased resolution • Structural selectivity through MS/MS Conclusion

59 Thank You for Your Attention! Questions? Stay connected with us Twitter @ChromSolutions Chromatography Solutions Blog http://chromblog.thermoscientific.com/blog YouTube http://www.youtube.com/ChromSolutions Facebook http://www.facebook.com/Chromatography Solutions Pinterest http://pinterest.com/chromsolutions/

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