2-(5-Benzoacridine)ethyl-p-toluenesulfonate as sensitive reagent for the determination of bile acids by HPLC with fluorescence detection and online atmospheric chemical ionization-mass spectrometric identification |
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Authors: | Jinmao You Yanyan Fu Zhiwei Sun Yourui Suo |
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Affiliation: | (1) Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining, 810001, China;(2) The Key Laboratory of Life-Organic Analysis, College of Chemistry Science, Qufu Normal University, Qufu Shandong, 273165, China;(3) Graduate University of the Chinese Academy of Science, Beijing, 100049, China |
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Abstract: | 2-(5-Benzoacridine)ethyl-p-toluenesulfonate (BAETS), a dual-sensitive probe, was reacted with bile acids in the presence of K2CO3 catalyst in dimethyl sulfoxide (DMSO) solvent to give BAETS–bile acid derivatives. Derivatives exhibited intense fluorescence (FL) with an excitation maximum at λ ex 270 nm and an emission maximum at λ em 510 nm. MS analysis using APCI-MS indicated that derivatives had excellent APCI-MS ionizability with percentage ionization δ values changing from 0 to 88.83% in aqueous acetonitrile and from 0 to 89.15% in aqueous methanol. The collision induced dissociation spectra of m/z [M + H]+ contained specific fragment ions at m/z [M + H−H2O]+, [M + H−2H2O]+, [M + H−3H2O]+, 347.3, and 290.1. Repeatability was good for LC separation of BAETS–bile acid derivatives with aqueous acetonitrile as mobile phase. The relative standard deviations (RSDs) of retention time and peak area at 6.6 nmol mL−1 levels with fluorescence detection (FL) were from 0.045 to 0.072% and from 2.16 to 2.73%, respectively. Excellent linear responses were observed, with regression coefficients >0.9995. The FL detection limits (S/N = 3) were in the range of 18.0–36.1 fmol. The online APCI-MS detection limits are in the range of 500–790 fmol (at a signal-to-noise ratio of 3). |
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