# US 11,307,183 B2 · Methods for determination of polar pesticides by chromatography > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,307,183 B2 - Document ID: US11307183B2 - Status: Granted - Kind: B2 - Application number: 16/514,347 - Filed: 2019-07-17 - Published: 2020-01-23 - Granted: 2022-04-19 - Earliest claimed: 2018-07-18 - Assignees: Waters Technologies Corporation - Applicants: Waters Technologies Corporation - Inventors: Danilo Augusto Alves Pereira; Mirela Talarico Afonso De Moura; Marcella Fernanda Alves Reis - Web page: https://patentgrep.com/patent/US11307183B2 ## CPC - G01N 30/88: Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 - B01J 20/287: Non-polar phases; Reversed phases - G01N 30/72: Mass spectrometers {(mass spectrometers per se H01J49/00)} - G01N 2030/027: {Liquid chromatography} - G01N 2030/884: {organic compounds} - G01N 2030/8845: {involving halogenated organic compounds} - G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS ## Abstract The disclosure relates to a reversed-phase chromatography method for the determination of at least one of glyphosate or AMPA in a sample. The method includes obtaining the sample comprising the at least one of glyphosate or AMPA in a sample matrix and introducing the sample to a reversed-phase chromatography system. The reversed-phase chromatography system includes a reversed-phase column having a stationary phase material contained inside the column. The stationary phase material includes a phenyl functional group. The method also includes flowing the sample with a mobile phase eluent through the reversed-phase column, wherein the at least one of glyphosate or AMPA is substantially resolved and retained. The mobile phase eluent has a pH between about 1.5 to about 2.5. The at least one of glyphosate or AMPA are detected using a detector. ## Claims ### Claim 1 A reversed-phase chromatography method for the determination of glyphosate or AMPA in a sample, the reversed-phase chromatography method comprising: obtaining the sample comprising at least one of glyphosate or AMPA in a sample matrix; introducing the sample to a reversed-phase chromatography system comprising a reversed-phase column having a stationary phase material contained inside the column, the stationary phase material comprising a phenyl functional group; flowing the sample with a mobile phase eluent through the reversed-phase column, wherein the at least one of glyphosate or AMPA is substantially resolved and retained, the mobile phase eluent having a pH between about 1.5 to about 2.5; and detecting the at least one of glyphosate or AMPA using a detector. ### Claim 2 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the pH of the mobile phase eluent is about 2. ### Claim 3 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the stationary phase material comprises a fluoro-phenyl functional group. ### Claim 4 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the stationary phase material comprises inorganic/organic hybrid particles. ### Claim 5 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the stationary phase material comprises ethylene bridged hybrid particles. ### Claim 6 (depends on 1) The reversed-phase chromatography method of claim 1, wherein obtaining the sample comprises extracting at least one of glyphosate or AMPA from food or soil to form an extract, wherein the extract is used as the sample. ### Claim 7 (depends on 6) The reversed-phase chromatography method of claim 6, wherein the at least one of glyphosate or AMPA is extracted using an organic solvent acidified with formic acid. ### Claim 8 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the sample comprises glyphosate and AMPA. ### Claim 9 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the mobile phase eluent comprises acetic acid. ### Claim 10 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the at least one of glyphosate or AMPA are separated in less than two minutes. ### Claim 11 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the AMPA is separated in less than one minute. ### Claim 12 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the detector is a mass spectrometer. ### Claim 13 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the mobile phase eluent has a flow rate between about 0.2 to about 1.0 mL/min. ### Claim 14 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the mobile phase eluent has a flow rate of about 0.40 mL/min. ### Claim 15 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the reversed-phase chromatography system is operated under isocratic conditions. ### Claim 16 (depends on 1) The reversed-phase chromatography method of claim 1, wherein the sample is a fruit sample, a vegetable sample or a soil sample. ### Claim 17 A kit comprising: (i) a reversed-phase chromatography system comprising (a) a reversed phase column having a stationary phase material contained inside the column, the stationary phase material comprising a phenyl functional group, and (b) a detector; and (ii) instructions contained in a computer readable medium for operating a reversed-phased chromatography system, wherein the instructions automate (a) introducing a sample to the reversed-phase chromatography system, the sample comprising at least one of glyphosate or AMPA; (b) flowing the sample with a mobile phase eluent through the reversed-phase column, wherein the at least one of glyphosate or AMPA is substantially resolved and retained, the mobile phase eluent having a pH between about 1.5 to about 2.5; and (c) detecting the at least one of glyphosate or AMPA using a detector. ### Claim 18 A kit comprising: (i) a reversed-phase chromatography column having a stationary phase material contained inside the column, the stationary phase material comprising a phenyl functional group; (ii) instructions contained in a computer readable medium for operating a reversed-phased chromatography system, wherein the instructions automate inserting a sample into a mobile phase eluent; flowing the sample with the mobile phase eluent through the reversed-phase chromatography column; and detecting components of the sample; and (iii) a vial containing the mobile phase eluent acidified to a pH of about 2.