The Evolution GC-MS/MS Triple Quadrupole System

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1 P.O. Box Alexandria, VA 22309, USA The Evolution GC-MS/MS Triple Quadrupole System Presented by Udo Rupprecht

2 Calgary Winter preferred over Australian Summer?(Strange)

3 Transforming the best GC-MS system into something even better!

4 Evolution on an Agilent 5975

5 TRIPLE QUADRUPOLE TECHNOLOGY ALL FUNCTIONS & ADVANTAGES OF MS/MS BASED ON AGILENT MSD 5975/B/C & 5973A/N CONTROLLED BY AGILENT MSD CHEMSTATION ALL DATA REDUCTION BY MSD CHEMSTATION UPGRADE YOUR OLD MSD TO A GC-MS/MS APPLICATIONS: FORENSIC SCIENCE DRUG TESTING RESIDUE IN FOOD DIOXIN TRACE ANALYSIS

6 Facts: The CHROMTECH EVOLUTION is built upon the most popular GC/MS-System, the AGILENT 5973/5975 series MSD. Uses the original inert ion source Uses the true hyperbolic quadrupole Uses the highly sensitive HED Uses original MSD Chemstation Additional IonRail collision cell and another high precision quadrupole - serving as mass filter Q3

7 Function and Advantages of Triple Quadrupole MS/MS: A triple quadrupole mass spectrometer (QqQ) links two stages of mass analysis. - Q1 pre-selects a precursor ion ( parent ion ) which is fragmented by collision with an inert gas in the RF-only collision cell (Q2). - The resulting product ( daughter ) ions are subsequently selected by the third quadrupole (Q3) mass filter. - Multiple Reaction Monitoring (MRM) is the most sensitive and selective technique to quantitate low levels of target compounds, especially in the presence of high background levels from sample matrix. Chemical background, usually present in single quad analysis (SIM), is almost completely eliminated.

8 CHROMTECH EVOLUTION GC-MS/MS System Mass Spectrometer Specifications Precursor (Parent), Neutral Loss, Single Reaction Monitoring (SRM), Mode (standard) EI Mode (optional) PCI, NCI, EI with CI source (5975) Ion source type Non-coated inert EI source (original 5973/75 ion source) Mass filter Q1: Monolithic hyperbolic quadrupole (original 5973/75 quadrupole) Q3: High-precision quadrupole with pre-and post filters Collision Cell Q2: 90 long path IonRail CID gas control Regulated via 6890 electronic pneumatic control (EPC) Mass range Up to 800 Da Detector EM with HED (original 5973/75 Detector) Scan modes Q1MS, Q3MS, Selected Ion Monitoring (SIM), Product (Daughter), Multiple Reaction Monitoring (MRM), Pumping system 250 L/s (5973) or 262 L/s (5975) turbomolecular

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11 Software is original Agilent MSD Chemstation with inserted macros for Q3 Autotune and other MS/MS control functions

12 Software is original Agilent MSD Chemstation with inserted macros for Q3 Autotune and other MS/MS control functions

13 Software is original Agilent MSD Chemstation with inserted macros for Q3 Autotune and other MS/MS control functions

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16 Applications

17 Analysis of Doping Confirmation Compounds Compounds RT MS/MS- Transitions SIM Trace Clenbuterol >300, Norandrosterone >227, Epimethendiol >225, Noretiocholanolone >315, Methyltestosterone M >301, Methyltestosterone M >225, Epimethandienone >315, α-Methyltestosterone (ISTD) >345,

18 Analysis of Doping Confirmation Compounds Linearity Test 8 point linearity study using 19- norandrosterone from 0.5 to 20ng/mL matrix R 2 = Figure 1: Linearity for 19-norandro-sterone with a concentration range from 0.5 to 20 ng/ml.

19 Analysis of Doping Confirmation Compounds Sensitivity RIC of Clenbuterol, Epimethendiole and 10- Noretiochola-none Figure 3: RIC of Clenbuterol, Epime-thendiole and 10-Noretiochola-none (all TMS derivatives) each 2 ng/ml. Despite the fact that the urinary matrix is sometimes visible, a good target and qualifier transition could be found in most cases.

20 Herbicides in Plants SIM Cleaned extract from Bell Pepper: Herbicide Dicofol searching with SIM ions m/z 111 and m/z 139 Retention time should be 9.05 minutes (as indicated). Identification and quantitation: Questionable

21 Herbicides in Plants SRM Same sample as above. Herbicide Dicofol searching with SRM m/z 139 > 111 Identification and quantitation: Easy, 50µg/ml

22 Herbicides in Plants Blue trace: SIM Black trace: SRM Cleaned extract from Bell Pepper: Blue trace, SIM Herbicide Tolylfluanid searching with SIM ion m/z 137 Maybe o.k. but confirmation needed! Black trace, SRM Herbicide Tolylfluanid searching with SRM m/z 238 > 137 Quantitation: 80 µg/ml Retention time should be 9.3 minutes as indicated with bar. Identification and quantitation on blue SIM trace: Questionable

23 Herbicides in Plants Confirmation needed for blue SIM trace: m/z 91: no confirmation possible Black SRM trace: 137 >91 Peak easily confirmed!

24 Differences From Other GC-MS/MS Systems Mass Stability approx. 0.1 amu in 48h Maintenance minimal compared to other MS/MS systems Chemstation software control Electronic Controlled Collision Gas (CID) 2 Filaments True Hyperbolic Quad Q1 heated up to 150 C

25 Future -NCI for OC Pesticides

26 Thank you for your kind attention.