Field sampling kit and methods for collecting and detecting alkyl methylphosphonic acids

Patent metadata

Field	Value
Publication number	US-10060887-B2
Application number	US-201113885634-A
Country	US
Kind code	B2
Filing date	Nov 15, 2011
Priority date	Nov 15, 2010
Publication date	Aug 28, 2018
Grant date	Aug 28, 2018

Abstract

The invention relates to kits and methods of collecting and detecting alkyl methylphosphonic acids from environmental or biological liquids using a sorbent material. The sorbent material may be transported, desorbed and tested for alkyl methylphosphonic acids.

First claim

We claim:

1. A method of collecting, from a liquid sample, a degradation product of an organophosphonate nerve agent, which consists of
adjusting the pH of the liquid sample to below about 3 with an acid having a pKa lower than 5;
adding a known amount of an isotopically labeled alkyl methylphosphonic acid to the liquid sample; and
performing solid phase microextraction by contacting the liquid sample having a pH below about 3 and the isotopically labeled alkyl methylphosphonic acid added thereto with a solid phase microextraction (SPME) fiber for a given period.

2. The method of claim 1 , wherein the given period is less than about 15 minutes.

3. The method of claim 1 , wherein the given period is about 1 minute to about 10 minutes.

4. A method of analyzing a degradation product of an organophosphonate nerve agent having been collected from a liquid sample by a collection method consisting of adjusting the pH of the liquid sample to below about 3 with an acid having a pKa lower than 5, adding a known amount of an isotopically labeled alkyl methylphosphonic acid to the liquid sample, and performing solid phase microextraction by contacting the liquid sample having a pH below about 3 and the isotopically labeled alkyl methylphosphonic acid added thereto with a solid phase microextraction (SPME) fiber, which said analyzing comprises
desorbing the degradation product from the SPME fiber after having been adsorbed thereon and stored for a given period; and
assaying the desorbed degradation product.

5. The method of claim 4 , wherein the desorbed degradation product is assayed using nuclear magnetic resonance, chromatography, mass spectrometry, or a combination thereof.

6. The method of claim 4 , wherein the desorbed degradation product is assayed using gas-chromatography-mass spectrometry (GC/MS), liquid chromatography-tandem mass spectrometry (LC/MS/MS), or high-performance liquid chromatography (HPLC).

7. The method of claim 4 , wherein the given period is greater than 3 months.

8. The method of claim 4 , wherein the given period is greater than 5 months.

9. The method of claim 1 , wherein the method is performed using a kit comprising
a solid phase microextraction (SPME) fiber;
a volumetric container;
an acid having a pKa lower than 5; and
an internal standard solution comprising a known amount of an isotopically labeled alkyl methylphosphonic acid.

10. The method of claim 9 , wherein the acid is acetic acid, formic acid, methane sulfonic acid, phosphoric acid, sulfuric acid, hydrochloric acid, hydrobromic acid, hydroiodic acid, trifluoromethane sulfonic acid, or toluenesulfonic acid.

11. The method of claim 9 , wherein the acid is provided in an amount of 50 μL to 3 mL.

12. The method of claim 9 , wherein the isotopically labeled alkyl methylphosphonic acid is present in a concentration of 100 ng/mL to 1 μl/mL.

13. The method of claim 9 , wherein the isotopically labeled alkyl methylphosphonic acid is pinacolyl methylphosphonic acid (PMPA), 2-(methyl)propyl methylphosphonic acid (MMPA), cyclohexyl methylphosphonic acid (CMPA), isopropyl methylphosphonic acid (IMPA), ethyl methylphosphonic acid (EMPA), or a combination of one or more thereof.

14. The method of claim 9 , wherein the SPME fiber comprises polydimethylsiloxane (PDMS), divinylbenzene (DVB), polyethylene glycol (PEG), octadecylsilyl (C 18 ), polyacrylate (PA), or a combination of one or more thereof.

15. The method of claim 9 , wherein the SPME fiber comprises a polyethylene glycol templated resin (CW/TPR) or octadecylsilyl (C 18 ).

16. The method of claim 9 , wherein the SPME fiber is provided as a retractable fiber assembly.

17. The method of claim 9 , wherein the SPME fiber is provided as a coating on the volumetric container.

18. The method of claim 9 , wherein the SPME fiber is attached to a cap for the volumetric container.

19. The method of claim 9 , wherein
the acid is acetic acid, formic acid, methane sulfonic acid, phosphoric acid, sulfuric acid, hydrochloric acid, hydrobromic acid, hydroiodic acid, trifluoromethane sulfonic acid, or toluenesulfonic acid;
the isotopically labeled alkyl methylphosphonic acid is pinacolyl methylphosphonic acid (PMPA), 2-(methyl)propyl methylphosphonic acid (MMPA), cyclohexyl methylphosphonic acid (CMPA), isopropyl methylphosphonic acid (IMPA), ethyl methylphosphonic acid (EMPA), or a combination of one or more thereof and is present in a concentration of 100 ng/mL to 1 μl/mL; and
the SPME fiber comprises polydimethylsiloxane (PDMS), divinylbenzene (DVB), polyethylene glycol (PEG), octadecylsilyl (C 18 ), polyacrylate (PA), or a combination of one or more thereof.

Assignees

• Lawrence Richard J
• Smith J Richard
• Capacio Benedict R
• Us Army

Inventors

• Lawrence Richard J
• Smith J Richard
• Capacio Benedict R

Classifications

• G01N1/10 Primary

  in the liquid or fluent state {(burettes, pipettes B01L3/02; sampling of ground water E02D1/06; metering by volume of fluids or fluent solid material G01F11/00, G01F13/00)} · CPC title

• B01J20/285

  based on polymers · CPC title

• B01J20/286

  Phases chemically bonded to a substrate, e.g. to silica or to polymers · CPC title

• G01N2001/149

  Capillaries; Sponges · CPC title

• Y10T436/163333

  Organic [e.g., chemical warfare agents, insecticides, etc.] · CPC title