Polar pesticide determination using chromatography

Patent metadata

Field	Value
Publication number	US-11092577-B2
Application number	US-201815914428-A
Country	US
Kind code	B2
Filing date	Mar 7, 2018
Priority date	Mar 8, 2017
Publication date	Aug 17, 2021
Grant date	Aug 17, 2021

Abstract

The present disclosure relates to the determination of pesticides, e.g., polar pesticides, in a sample using chromatography. The present disclosure can provide direct analysis of polar pesticides, including anionic polar pesticides, using high performance liquid chromatography. The polar pesticides are sufficiently retained and resolved to allow for multiple polar pesticide determinations in a single analysis.

First claim

We claim:

1. A chromatography method for determining at least one polar pesticide or metabolite, the method comprising:
(i) obtaining a sample containing at least one polar pesticide or metabolite in a sample matrix;
(ii) introducing the sample to a chromatography system comprising a column having a reverse phase stationary phase material contained inside the column, wherein the reverse phase stationary phase material comprises inorganic/organic hybrid particles, a diol functional group, and an amine functional group, wherein the ratio of amine functional group to diol functional group is between about 0.01:1 and 1:1, and wherein the reverse phase stationary phase material is configured to operate under a pressure at or above 1,000 psi;
(iii) flowing the sample with a mobile phase eluent through the column, wherein the at least one polar pesticide or metabolite is substantially resolved and retained; and
(iv) detecting the at least one polar pesticide or metabolite using a detector.

2. The method of claim 1 , wherein the sample contains at least 2 polar pesticides or metabolites and the at least 2 polar pesticides or metabolites are substantially resolved and retained.

3. The method of claim 1 , further comprising extracting the at least one polar pesticides or metabolite from the sample matrix before introducing the extracted sample to the chromatography system.

4. The method of claim 1 , wherein the at least one polar pesticide or metabolite is selected from the group consisting of Ethephon, Glufosinate-ammonium, Glyphosate, Fosetyl-aluminum, Phosphonic acid, Maleic hydrazide, Perchlorate, Chlorate, Cyromazine, Amitrole, Daminozide, Ethylenethiorea, Propylenethiourea, Chlormequat, Mepiquat, Diquat, Paraquar, and metabolites thereof, and combinations thereof.

5. The method of claim 1 , wherein the amine functional group comprises a diethyl amine functional group, a 2-picoylamine functional group, a 2-ethylpyridine functional group, or a 4-ethylpyridine functional group.

6. The method of claim 1 , wherein the mobile phase eluent comprises acetonitrile, buffer or combinations thereof.

7. The method of claim 1 , wherein the mobile phase eluent has a flow rate between 0.2 and 1.0 mL/min.

8. The method of claim 1 , wherein the mobile phase eluent comprises organic and aqueous solvents containing buffer, or combinations thereof, and wherein the at least one polar pesticide or metabolite is eluted using a gradient elution, the elution comprising a gradient of a first solvent comprising an aqueous solvent and a second solvent comprising an organic solvent.

9. The method of claim 1 , wherein the column temperature is between 30 and 60° C.

10. The method of claim 1 , wherein the method repeatability of performing the method of claim 1 at least 10 times using the same chromatography system measuring peak area has a Relative Standard Deviation (RSD) of less than about 20%, wherein the sample is a solution of polar pesticide or metabolite reference standards.

11. The method of claim 1 , wherein the sample contains at least 2 polar pesticides or metabolite which are substantially resolved, and wherein the substantially resolved at least 2 polar pesticides or metabolites have a resolution greater than 1.

12. The method of claim 1 , wherein the detector is selected from the group consisting of a UV/VIS detector, PDA detector, fluorescence detector, mass spectrometer, refractive index detector, evaporative light scattering detector and a charged aerosol detection.

13. The method of claim 1 , wherein the amine functional group is a diethyl amine functional group.

14. The method of claim 1 , wherein the retention time for the at least one polar pesticide or metabolite is at least twice the retention time corresponding to the void volume of the column.

15. The method of claim 8 , wherein:
the first solvent is 50 mM ammonium formate in water, adjusted to pH 2.9 with formic acid; and
the second solvent is 0.9% formic acid in acetonitrile.

16. The method of claim 15 , wherein the gradient comprises an initial ratio of the first solvent to the second solvent of 10:90, increasing to a ratio of the first solvent to the second solvent of 60:40 over a first period of time.

17. The method of claim 16 , wherein the first period of time is 4.5 minutes.

18. The method of claim 16 , further comprising continuing the elution at the 60:40 ratio of the first solvent to the second solvent for a second period of time.

19. The method of claim 1 , further comprising:
(v) washing the column with an aqueous solution of 0.5 to 10 mM citric acid, followed by washing the column with a solution of formic acid in acetonitrile.

20. The method of claim 1 , wherein the at least one polar pesticide is anionic.

Assignees

• Waters Technologies Corp

Inventors

• Shah Dimple D
• Fairchild Jacob N
• Ross Euan
• Wuyts Benjamin

Classifications

• G01N30/88 Primary

  Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 · CPC title

• G01N30/74

  Optical detectors {(measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J)} · CPC title

• G01N30/72

  Mass spectrometers {(mass spectrometers per se H01J49/00)} · CPC title

• G01N30/8631

  Peaks · CPC title

• G01N2030/884

  organic compounds · CPC title