US 11,940,429 B2
Methods for authenticating botanicals using a marker compound's related chromatographic profile and mass spectral profile jointly
Jinchuan Yang, Hopkinton, MA (US); and Paul Rainville, Princeton, MA (US)
Assigned to Waters Technologies Corporation, Milford, MA (US)
Filed by Waters Technologies Corporation, Milford, MA (US)
Filed on May 1, 2019, as Appl. No. 16/400,163.
Claims priority of provisional application 62/665,727, filed on May 2, 2018.
Prior Publication US 2019/0339238 A1, Nov. 7, 2019
Int. Cl. G01N 30/86 (2006.01); G01J 3/00 (2006.01); G01N 30/02 (2006.01); G01N 30/72 (2006.01); G01N 30/74 (2006.01); G01N 33/00 (2006.01); G01R 33/46 (2006.01)
CPC G01N 30/8675 (2013.01) [G01J 3/00 (2013.01); G01N 30/72 (2013.01); G01N 30/74 (2013.01); G01N 33/0098 (2013.01); G01R 33/46 (2013.01); G01N 2030/025 (2013.01); G01N 2030/027 (2013.01)] 18 Claims
OG exemplary drawing
 
1. A method for authenticating a botanical comprising:
identifying at least one marker compound of the botanical;
injecting a sample comprising the botanical into a chromatography system comprising a mobile phase delivery module, an autosampler, a chromatography column, a chromatography column manager, and a data acquisition module in communication with at least one detector comprising a mass spectrometer, wherein the data acquisition module is a computer having software installed to collect and analyze data received from the detector;
extracting a chromatogram of the at least one marker compound, the extracted chromatogram comprising at least one peak;
extracting a mass spectrum at a chromatographic peak retention time of the at least one marker compound, the extracted spectrum comprising at least one band;
integrating the at least one peak of the extracted chromatogram to determine a marker compound peak relative area using the data acquisition module;
quantifying the at least one peak of the extracted chromatogram;
quantifying the at least one band of the extracted mass spectrum;
comparing the quantified at least one peak of the extracted chromatogram to an authentic sample chromatogram and the quantified at least one band of the extracted mass spectrum to an authentic sample mass spectrum at the same time wherein the sample is authenticated by an authentication protocol comprising determining (a) whether the at least one peak of the extracted chromatogram is detected within a peak retention window of an at least one peak of the authentic sample chromatogram, (b) whether the marker compound peak relative area is within threshold limits of a marker compound peak relative area of the authentic sample mass spectrum, (c) whether the mass spectrum is matched in a spectrum library, and (d) whether an ion relative abundance of the at least one band of the extracted mass spectrum is within threshold limits of an ion relative abundance of the authentic mass spectrum, wherein the software automates the authenticity data process protocol, and wherein the botanical is authenticated when all values of the quantified at least one peak and the quantified at least one band are within the predetermined standard deviation or percentage threshold value and the extracted mass spectrum matches the predetermined mass spectrum.