Enhancing Utility and Throughput of SPME using Advanced Automation Strategies

Transcription

1 Supelco Innovation Seminars November 11 th, 2010 Atlanta, GA Enhancing Utility and Throughput of SPME using Advanced Automation Strategies Presented by Tom Tobien, Ph.D. Analytical Chemist, LEAP Technologies, Carrboro, NC

2 The LEAP CTC CombiPAL Autosampler Platform: Main Design Features: Direct Automation of Manual Steps 2

3 The LEAP CTC CombiPAL Autosampler Platform: Main Design Features: Versatility 3

4 The Way to Accomplish Versatility Accessories - Trays 4

5 The Way to Accomplish Versatility Accessories Sample Cooling 5

6 The Way to Accomplish Versatility Accessories Custom Trays 6

7 The Way to Accomplish Versatility Accessories Headspace Option Example: 2.5mL Headspace (HS) Syringe & HS Upgrade Kit 7

8 The Way to Accomplish Versatility Accessories Liquid Injection & SPME Option Example: 10μL Liquid Injection Syringe Example: SPME Fiber Holder 8

9 The SPME Kit for the CombiPAL 9

10 The SPME Fiber Conditioner Accessory Fiber Heating in Inert Gas Stream Beneficial for Initial Conditioning of New Fibers Can Heat at Higher/Different Temperature Than GC Inlet Also Called Needle Heater 10

11 CombiPAL Standard SPME Operation Movie Clip (A short movie clip depicting all CombiPAL autosampler steps during SPME fiber sampling and SPME desorption into a GC inlet is being shown. The movie clip is not embedded into presentation.) 11

12 Automated Standard SPME Applications Excellent Supelco Library of Manual Applications Easily Converted into Automated CombiPAL Procedure Headspace & Liquid Phase Fiber Extractions (Keyword: Vial Penetration Depth) 10 and 20mm Fiber Lengths Likely Need for Internal Standard Due to Fiber Extraction Selectivity, e.g., Deuterated Analytes, Matrix-Dependent 12

13 Automated Standard SPME Applications Standard Setup Example with Space Constraints 13

14 Examples for Automated Standard SPME Applications US EPA Method 8272: PAHs in Sediment Pore Water by SPME and GC/MS (SIM) Reference: US EPA Method 8272 Rev 0, December /sw846/new_meth.htm#

15 Examples for Automated Standard SPME Applications US EPA Method 8272: PAHs in Sediment Pore Water by SPME and GC/MS (SIM) Reference: US EPA Method 8272 Rev 0, December /sw846/new_meth.htm#

16 Examples for Automated Standard SPME Applications CDC Method Trihalomethanes and MTBE in Ground Water by SPME and GC/MS (Isotope Dilution) Reference: CDC Method THMs and MTBE VOCs in Water, NCEH/DLS/ERAT, DLS Method Code: VO-BTHM-1.01, rev. Jan 6, s_05_06/l04voc_d_met_%20voc_water.pdf 16

17 Examples for Automated Standard SPME Applications CDC Method Volatile Organic Compounds in Whole Blood by SPME and GC/MS (Isotope Dilution) Reference: CDC Method Volatile Organic Compounds in Whole Blood, NHNANES , Method Code: 13-OD; VO-BTHM s_03_04/l04voc_c_met_blood.pdf 17

18 Advanced Automation of SPME Applications Almost Always Requires a Twin-Headed PAL Autosampler Version 1 Dual-SPME Fiber Extraction (1 per Head) Version 2 Sample Preparation Prior to SPME Head #1 = SPME Fiber Head #2 = Sample Preparation/Manipulation Exception: Internal Standard Dispense into Vial via Tool 18

19 Advanced Automation of SPME Applications Internal Standard Dispense into Vial via LEAP Dispense Tool PAL Injection Head with Bracket to Pickup Dispense Tool Metering Pump Connected to Tool Ability to Penetrate Septa 19

20 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction (1 SPME Fiber per PAL Head) Objective: Increase Throughput Staggered Sampling & GC Inlet Desorption Additional Events Scheduling Software Required 20

21 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction (1 SPME Fiber per PAL Head) 21

22 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction - Chronos Events Scheduling Software 22

23 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction - Chronos Events Scheduling Software Sample Pre- Incubation Fiber Extraction Fiber Desorption & Conditioning GC Cooldown Put Vial in Incubator Expose Fiber to Headspace Expose Fiber in GC Inlet Retract Fiber & Return Vial 23

24 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction - Chronos Events Scheduling Software 24

25 Advanced Automation of SPME Applications Dual-SPME Fiber Extraction Target Application CDC Method: Mercury in Whole Blood 25

26 Advanced Automation of SPME Applications Sample Preparation Prior to SPME Head #1 = SPME Fiber Head #2 = Sample Preparation/Manipulation Objective: Increase Throughput by Automation of Sample Preparation Procedures (Part or Whole) Staggering of Sample Prep & Fiber Extraction/Desorption Just-in-Time Sample Prep Additional Events Scheduling Software Required 26

27 Advanced Automation of SPME Applications Sample Preparation Prior to SPME, e.g., Derivatization Incubation IS Addition Mixing 27

28 Advanced Automation of SPME Applications Sample Preparation Prior to SPME Additional Options: Filtration SPE Extraction 28

29 Next Frontiers in Advanced SPME Automation Automated Fiber Exchange 29

30 Next Frontiers in Advanced SPME Automation Coupling SPME Fiber Desorption with LC With Permission from K. Furton, Florida International University, Miami, FL Reference: Furton KG, Wu L, Almirall JR. Optimization of solid-phase microextraction (SPME) for the recovery of explosives from aqueous and post-explosion debris followed by gas and liquid chromatographic analysis. J Forensic Sci 2000;45(4):

31 Special Thanks Goes To: Mark Fresquez, CDC Atlanta, GA, for permission to talk about the Dual-SPME TwinPAL setup Brian Peat & Steven Stiller, LEAP Technologies, for valuable contributions to this presentation Supelco for the invitation to present this talk. and to you for your attention! 31