System and method for desorbing and detecting an analyte sorbed on a solid phase microextraction device

• US 10,429,362 B2
• Filed: 10/16/2018
• Issued: 10/01/2019
• Est. Priority Date: 05/10/2016
• Status: Active Grant

• Current Assignee: JP Scientific Limited
• Original Assignee: JP Scientific Limited
• Inventors: Pawliszyn, Janusz B.
• Primary Examiner(s): Wecker, Jennifer
• Application Number:
  US16/162,034
• Publication Number:
  US 20190049415A1
• Time in Patent Office: 350 Days
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 1/44 Sample treatment involving radiation, e.g. heat
• CPC Class Codes: G01N 2001/1445 Overpressure, pressurisation at sampling point
• CPC Class Codes: G01N 2030/009 Extraction
• CPC Class Codes: G01N 2030/062 extracting sample from raw material
• CPC Class Codes: G01N 21/714 Sample nebulisers for flame burners or plasma burners nebulizers per se B05B
• CPC Class Codes: G01N 2560/00 Chemical aspects of mass spectrometric analysis of biological material
• CPC Class Codes: G01N 30/00 Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation G01N3/00, G01N5/00, G01N7/00, G01N9/00, G01N11/00, G01N13/00, G01N15/00, G01N17/00, G01N19/00, G01N21/00, G01N22/00, G01N23/00, G01N24/00, G01N25/00, G01N27/00, G01N29/00 take precedence
• CPC Class Codes: G01N 30/06 Preparation
• CPC Class Codes: G01N 30/7266 by electric field, e.g. electrospray
• CPC Class Codes: H01J 49/0431 for liquid samples interfaces to liquid chromatographs G01N30/7233
• CPC Class Codes: H01J 49/0459 for solid samples

Abstract

Disclosed herein is a system for desorbing and detecting an analyte sorbed on a solid phase microextraction (SPME) device. The system includes a desorption chamber sized to accept the SPME device while defining a void volume of less than about 50 μL; a flow injector in fluid connection with the desorption chamber, the desorption chamber and the flow injector being fluidly connected by at least a flow-insulating fluid connector; a solvent source in fluid connection with the flow injector; and a fluid switch that: in a desorption position, allows the solvent to be sprayed from the flow injector while flow-insulating any desorption solution in the desorption chamber, and in an detecting position, turns off the solvent source while maintaining the fluid connection between the flow injector and the desorption chamber, transferring the desorption solution through the flow-insulating fluid connector to the flow injector as a substantially undiluted plug of liquid.

Claims

1. A system for desorbing and detecting an analyte sorbed on a solid phase microextraction (SPME) device, the system comprising:

a desorption chamber configured to be open to atmospheric pressure during operation and sized to accept the SPME device while defining a void volume of less than about 50 μ

L;

a flow injector in fluid connection with the desorption chamber, the desorption chamber and the flow injector being fluidly connected by at least a flow-insulating fluid connector;

a solvent source in fluid connection with the flow injector; and

a fluid switch that;

(a) in a desorption position, is configured to allow the solvent to be sprayed from the flow injector while flow-insulating any desorption solution in the desorption chamber, and

(b) in an detecting position, is configured to isolate the solvent source from the flow injector by turning off the solvent flow while maintaining the fluid connection between the flow injector and the desorption chamber so as to transfer desorption solution in the desorption chamber through the flow-insulating fluid connector to the flow injector as a substantially undiluted plug of liquid.

2. The system according to claim 1, wherein the flow-insulating fluid connector is dimensioned to reduce or avoid diffusion of desorption solution from the desorption chamber to the solvent flowing to the flow injector when (a) the fluid switch is in the desorption position, and (b) the solvent flows from the solvent source to the flow injector.

3. The system according to claim 2, wherein:

the flow-insulating fluid connector has a smaller cross-section than a cross-section of the desorption chamber;

the length of the flow-insulating flow connector is sufficiently greater than the cross-section of the flow flow-insulating connector that liquid flowing past one end of the fluid connector does not affect liquid at the other end of the fluid connector;

or both.

4. The system according to claim 1, wherein the flow-insulating fluid connector is sized to be fluidly blocked by an accepted SPME device, fluidly isolating the desorption chamber from the flow injector during desorption.

5. The system according to claim 4, further comprising at least one additional desorption chamber sized to accept the SPME device while defining a void volume of less than about 50 μ

L, wherein the additional desorption chamber;

is connected in parallel to the other desorption chamber, is fluidly connected to an additional flow-insulating fluid connector that is sized to be fluidly blocked by an additional accepted SPME device, and is fluidly connected to the flow injector when the additional SPME device is not fluidly blocking the additional flow-insulating fluid connector.

6. The system according to claim 1, wherein the system includes a detection device at a lower pressure than the desorption chamber, and the flow injector is an electrospray needle, a thermospray nebulizer, a microelectrospray needle, an atmospheric pressure chemical ionization nebulizer, an ion-mobility spectrometry nebulizer, an inductively coupled plasma nebulizer, or a system that produces a pressure deferential that drives the solvent flow towards the detection device.

7. The system according to claim 6 wherein the detection device is a mass spectrometer, ion mobility spectrometer, or electrochemical or optical spectroscopy-based detector downstream of the flow injector for detecting the desorbed analyte.

8. The system according to claim 1, wherein the solvent source is fluidly connected with the flow injector at least through a pump capable of applying a pressure to the solvent to transfer the solvent to the flow injector.

9. The system according to claim 1, further comprising a gas source for nebulizing solvent flowing from the flow injector.

10. The system according to claim 1, further comprising an agitator to vibrate an accepted SPME device, a heater to heat the desorption chamber, or both.

11. A system for desorbing and detecting an analyte sorbed on a solid phase microextraction (SPME) device, the system comprising:

a desorption chamber sized to accept the SPME device while defining a void volume of less than about 50 μ

L;

a flow injector in fluid connection with the desorption chamber, the desorption chamber and the flow injector being fluidly connected by at least a flow-insulating fluid connector;

a solvent source in fluid connection with the flow injector;

a 3-way junction fluidly connecting (1) the desorption chamber, (2) the solvent source, and (3) the flow injector; and

a fluid switch that;

(a) in a desorption position, allows the solvent to be sprayed from the flow injector while flow-insulating any desorption solution in the desorption chamber, and

(b) in an detecting position, isolates the solvent source from the flow injector by turning off the solvent flow while maintaining the fluid connection between the flow injector and the desorption chamber so as to transfer desorption solution in the desorption chamber through the flow-insulating fluid connector to the flow injector as a substantially undiluted plug of liquid;

wherein, during operation, the desorption chamber is configured to be open to atmospheric pressure and the flow injector is at a reduced pressure in comparison to the solvent source and the desorption chamber;

wherein, during operation, the desorption chamber is arranged to reduce or prevent fluid from dripping out of the desorption chamber; and

wherein the fluid switch is configured to change the relative flows of (a) fluid from the solvent source to (b) fluid drawn from the flow injector.

12. The system according to claim 11, wherein:

(a) the 3-way junction flow-insulates the desorption solution in the desorption chamber when the fluid switch is set to allow substantially the same flow rate from the solvent source as the flow rate from the flow injector,

(b) the 3-way junction allows the transfer of the desorption solution in the desorption chamber to the flow injector when the fluid switch is set to allow a reduced flow rate from the solvent source than the flow rate from the flow injector, and

(c) the 3-way junction allows the transfer of the desorption solution in the desorption chamber to the flow injector when the fluid switch is set to allow an greater flow rate from the solvent source than the flow rate from the flow injector.

13. The system according to claim 11, wherein the desorption chamber is a portion of tubing connected to the 3-way junction.

14. The system according to claim 11, wherein the 3-way junction is a chromatographic T-junction.

15. The system according to claim 11, wherein the fluid switch is a valve fluidly located between the solvent source and the 3-way junction.

16. A method for desorbing and detecting an analyte sorbed on a solid phase microextraction (SPME) device, the method comprising:

desorbing at least some of the analyte from the SPME device into a desorption solution in a desorption chamber that is in fluid connection with a flow injector, wherein the desorption solution in the desorption chamber is substantially not flowing to the flow injector;

nebulizing a solvent from the flow injector while the analyte is desorbing into the desorption solution in the desorption chamber, wherein the solvent is nebulized from the flow injector at a rate sufficient to fluidly isolate the desorption solution in the desorption chamber from the solvent being nebulized;

flushing substantially all of the desorption solution in the desorption chamber to the flow injector as a substantially undiluted plug of liquid; and

spraying the desorption solution through the flow injector into a detection device.

17. The method according to claim 16, further comprising applying pressure to the solvent using a pump to transfer the solvent from a solvent source to the flow injector.

18. The method according to claim 16, wherein the desorption solution in the desorption chamber is flushed to the flow injector by (a) reducing the flow rate of solvent provided to the flow injector, or (b) fluidly isolating the flow injector from the solvent source, thereby hydrodynamically driving the desorption solution in the desorption chamber to the flow injector by suction generated by a nebulizing gas.

19. The method according to claim 18, further comprising refilling the desorption chamber by increasing the flow rate of solvent provided to the flow injector in comparison to the flow rate of solvent being nebulized, or decreasing the flow rate of solvent being nebulized in comparison to the flow rate of solvent provided to the flow injector.

20. The method according to claim 16, wherein the desorption chamber is not in fluid connection with the flow injector while the analyte is desorbing into the desorption solution in the desorption chamber, and flushing the desorption solution in the desorption chamber to the flow injector comprises making a fluid connection between the desorption chamber and the flow injector.

21. The method according to claim 20, wherein the SPME device breaks the fluid connection between the desorption chamber and the flow injector while the analyte is desorbing from the SPME device by blocking an aperture fluidly connected to the flow injector, and making the fluid connection between the desorption chamber and the flow injector comprises unsealing the aperture.

22. The method according to claim 21, further comprising removing the SPME device from the desorption chamber and inserting another SPME device into the desorption chamber to block the aperture.

23. The method according to claim 20, further comprising desorbing, flushing, and spraying an analyte from at least one additional SPME device, wherein the desorbing of the analytes from the SPME device and from the at least one additional SPME device is performed in parallel.

24. The method according to claim 16, wherein the flow injector is an electrospray needle, a thermospray nebulizer, a microelectrospray needle, an atmospheric pressure chemical ionization nebulizer, an ion-mobility spectrometry nebulizer, an inductively coupled plasma nebulizer, or a system that produces a pressure deferential that drives the solvent flow towards the detection device.

25. The method according to claim 16, wherein the detection device is a mass spectrometer, an ion mobility spectrometer, or an electrochemical or optical spectroscopy-based detector.

26. The method according to claim 16, further comprising heating the desorption chamber, vibrating the SPME device, or both.