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Liquid Chromatography/Mass Spectrometry with Atmospheric Pressure Chemical Ionization of Free Brassinosteroids
Author(s) -
Gamoh Keiji,
Abe Hiroyuki,
Shimada Katsuya,
Takatsuto Suguru
Publication year - 1996
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/(sici)1097-0231(19960610)10:8<903::aid-rcm564>3.0.co;2-2
Subject(s) - chemistry , atmospheric pressure chemical ionization , mass spectrometry , brassinolide , chemical ionization , chromatography , ion , mass spectrum , analytical chemistry (journal) , polyatomic ion , atmospheric pressure , acetonitrile , detection limit , ionization , high performance liquid chromatography , organic chemistry , plant growth , botany , oceanography , biology , geology
Liquid chromatography/mass spectrometry (LC/MS) with atmospheric pressure chemical ionization has been successfully applied to the simultaneous analysis of free brassinosteroids (polyhydroxylated steroids that serve as plant growth regulators) as their naphthaleneboronates. Of a range of analytical conditions that were tested, optimum results were obtained by the use of reversed‐phase high‐performance liquid chromatography using a mixture of acetonitrile and water. The positive‐ion spectra of naphthaleneboronates of brassinosteroids showed pseudo‐molecular ions, [M+H] + , and fragment ions corresponding to the losses of hydroxyl groups of the steroidal nucleus. The [M+H] + ion was the most abundant for brassinolide and the [M+H−H 2 O] + ions were the most abundant for castasterone, teasterone and typhasterol. Full‐scan mass spectra were readily obtained from 400 ng of free brassinosteroids, while a limit of detection of 2 ng (signal‐to‐noise ratio 3) was attained in the selected‐ion monitoring mode. The application of LC/MS to the study of brassinosteroids in a plant material is demonstrated by the analysis of seeds of Cannabis sativa L.