# US 12,191,133 B2 · Mass spectrometry method for identifying and/or authenticating a sample > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 12,191,133 B2 - Document ID: US12191133B2 - Status: Granted - Kind: B2 - Application number: 17/610,010 - Filed: 2020-05-08 - Published: 2022-06-23 - Granted: 2025-01-07 - Earliest claimed: 2019-05-10 - Assignees: Orvinum AG - Applicants: Orvinum AG - Inventors: Frank Jochen Dieterle; Timm Fabian Manfred Hettich; Christian Berchtold; Gotz Schlotterbeck; Markus Ehrat - Web page: https://patentgrep.com/patent/US12191133B2 ## CPC - G01N 33/6848: {Methods of protein analysis involving mass spectrometry} - H01J 49/165: {Electrospray ionisation} - G01N 33/94: involving narcotics {or drugs or pharmaceuticals, neurotransmitters or associated receptors} - H01J 49/0036: {Step by step routines describing the handling of the data generated during a measurement} - G01N 33/146: {containing alcohol} - G01N 33/4833: {of solid biological material, e.g. tissue samples, cell cultures (tissue in vivo A61B5/00; cell suspensions G01N33/48735)} - G01N 33/49: Blood {(chemical methods for determining blood cell populations G01N33/5094; chemical analysis of blood groups or blood types G01N33/80)} - G01N 33/493: urine - 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) - H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H) ## Abstract The present invention relates to a method for identifying and/or authenticating a sample, comprising adding at least one chemical compound to the sample, determining a level of the at least one compound after addition to the sample; comparing the level of the at least one compound to a reference level and identifying the sample based on the comparison with the reference sample and the effect of the sample on the level of the at least one compound. The invention further relates to the use of the at least one compound in the method for identifying and/or authenticating a sample. Further, the invention relates to the use of a kit comprising the at least one compound in the inventive method. In addition, the invention relates to a composition comprising the at least one compound. Further, the invention relates to a kit comprising the compositions provided herein, e.g. for calibrating the methods provided herein and/or the instruments employed in the methods provided herein. ## Claims ### Claim 1 A method for identifying and/or authenticating a sample, wherein the method comprises the steps of: (i) adding at least one compound to the sample, wherein the at least one compound has a variable ionization; (ii) obtaining a mass spectrum of the at least one compound and determining a level of the at least one compound after addition to the sample; (iii) comparing the level of the at least one compound determined in (ii) to a reference level, wherein the reference level is a level of the same compound determined after addition to a reference sample; and (iv) identifying the sample based on the comparison in step (iii) and the effect of the sample on the level of the at least one compound. ### Claim 2 (depends on 1) The method of claim 1, wherein the level is (a) mass spectrometry signal level(s), in particular wherein the level is the abundance determined in the mass spectrum. ### Claim 3 (depends on 1) The method according to claim 1, wherein the sample has an ion suppression, or has an ion enhancement effect on the at least one compound or wherein the sample does not substantially alter the ionization of the at least one compound. ### Claim 4 (depends on 1) The method according to claim 1, wherein the ion suppression efficiency or the ion enhancement efficiency of the sample on the at least one compound is determined, and said ion suppression efficiency or said ion enhancement efficiency is compared to the ion suppression efficiency or to the ion enhancement efficiency of the reference sample on the same at least one compound, and based thereon the sample is identified. ### Claim 5 (depends on 1) The method according to claim 1, wherein a similar or an identical level of the at least one compound compared to the reference level indicates that the sample corresponds to the reference sample; or wherein a difference in the level of the at least one compound as compared to the reference level indicates that the sample does not correspond to the reference sample. ### Claim 6 (depends on 1) The method according to claim 1, wherein in step (iv) the sample is identified based on the particular pattern of ion suppression or ion enhancement of the at least one compound. ### Claim 7 (depends on 1) The method according to claim 1, wherein a sample is used in step (i) without experiencing a separation step, suitably such that the level(s) in step (ii) are determined without a chromatographic separation, and preferably wherein the mass spectrum is obtained by a mass spectrometer coupled to an ion source, in particular an electrospray ionization. ### Claim 8 (depends on 1) The method according to claim 1, wherein in step (i) different concentrations of the at least one compound are added to the sample, and wherein in step (ii) the levels of the different concentrations of the at least one compound after addition to the sample are determined; or wherein in step (i) the at least one compound is added to different concentrations of the sample and wherein in step (ii) the levels of the at least one compound after addition to the samples are determined. ### Claim 9 (depends on 1) The method according to claim 1, wherein the method comprises to generate a dose response curve, in particular wherein the dose response curve is based on the levels of different concentrations of the at least one compound; or wherein the dose response curve is based on the levels of the at least one compound after addition to said different concentrations of said sample. ### Claim 10 (depends on 1) The method according to claim 1, wherein in step (i) 1 to 100 compounds are added. ### Claim 11 (depends on 1) The method according to claim 1, wherein the compounds are susceptible to an ion suppression and/or ion enhancement effect of particular substances comprised in the sample. ### Claim 12 (depends on 1) The method according to claim 1, wherein the compounds are distinguishable in the mass spectrum. ### Claim 13 (depends on 1) The method according to claim 1, wherein the compounds have a high or low molecular weight, a different partition coefficient (log P), and/or a different pka. ### Claim 14 (depends on 1) The method according to claim 1, wherein in step (ii) the level of each of the at least one compound is determined, and wherein in step (iii) the level of each of the at least one compound is compared to each reference level. ### Claim 15 (depends on 1) The method according to claim 1, wherein the at least one compound is not comprised in the sample. ### Claim 16 (depends on 1) The method according to claim 1, wherein the at least one compound is selected from the group consisting of sulfaguanidine, naproxen sodium, sulfadimethoxine, ciprofloxacin, tetracycline hydrochloride, verapamil hydrochloride, terfenadine, leucine enkephalin acetate salt hydrate and reserpine. ### Claim 17 (depends on 1) The method according to claim 1, wherein the at least one compound has a concentration in the sample of at least 5 times the limit of quantification after addition to the sample. ### Claim 18 (depends on 1) The method according to claim 1, wherein the at least one compound has a concentration in the sample after addition to the sample to suppress and/or enhance the level of the least one compound to about 20% to about 80% in comparison to the level of the same compound determined in the absence of the sample. ### Claim 19 (depends on 1) The method according to claim 1, wherein further levels of a standard are determined, in particular for calibrating the method of any of the preceding claims. ### Claim 20 (depends on 1) The method according to claim 1, wherein the sample is a pooled sample suitable for the use in quality control. ### Claim 21 (depends on 1) The method according to claim 1, wherein the sample is selected from the group consisting of wine, spirituous beverage, foodstuff, processed foodstuff, tea, coffee, herb extract, natural product, natural products extracts, beer, fruit juice (for example orange and apple), a pharmaceutical composition, a formulation of a pharmaceutical, a body fluid, tissue extract, blood, blood plasma, blood serum, and urine. ### Claim 22 (depends on 1) The method according to claim 1, wherein the reference sample allows the identification and/or authentication of the sample. ### Claim 23 (depends on 1) The method according to claim 1, wherein the sample and the reference sample are from the same sort. ### Claim 24 (depends on 1) The method according to claim 1, wherein the reference sample is an authentic sample or a sample with a known composition. ### Claim 25 (depends on 1) The method according to claim 1, wherein the reference sample is a wine sample of particular vintage, of a particular grape variety, or from a particular region, or from a particular producer. ### Claim 26 (depends on 1) The method according to claim 1, wherein the identification of the sample is the identification of a dilution of the sample, in particular wherein the dilution of the sample is identified based on the comparison of the dose response curve of the sample to the dose response curve of the reference sample, in particular wherein the dose response curves are based on the levels of the different concentrations of the at least one compound or the level of a constant concentration of the at least one compound. ### Claim 27 (depends on 1) The method according to claim 1, wherein the method comprises a calibration step, wherein the sample comprises known compounds with known variable ionization and/or known ionization effects, such as a known ion suppression effect on the at least one compound, a known ion enhancement effect on the at least one compound or known to not substantially alter the level of the at least one compound, and wherein the sample is used to calibrate the method and/or the instruments employed in any one of the preceding claims.