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.
2-(5-Benzoacridine)ethyl-p-toluenesulfonate (BAETS), a dual-sensitive probe, was reacted with bile acids in the presence of K(2)CO(3) catalyst in dimethyl sulfoxide (DMSO) solvent to give BAETS-bile acid derivatives. Derivatives exhibited intense fluorescence (FL) with an excitation maximum at lambda(ex) 270 nm and an emission maximum at lambda(em) 510 nm. MS analysis using APCI-MS indicated that derivatives had excellent APCI-MS ionizability with percentage ionization delta 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-H(2)O](+), [M + H-2H(2)O](+), [M + H-3H(2)O](+), 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).
Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001, China. Jmyou6304@163.com
Jinmao
J
You
Yanyan
Y
Fu
Zhiwei
Z
Sun
Yourui
Y
Suo
D000166:Acridines / Q000737:chemistry*; D001274:Atmospheric Pressure; D001557:Benzenesulfonates / Q000737:chemistry*; D001647:Bile Acids and Salts / Q000032:analysis* / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007202:Indicators and Reagents / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
C550376:2-(5-benzoacridine)ethyl-p-toluenesulfonate; D000166:Acridines; D001557:Benzenesulfonates; D001647:Bile Acids and Salts; D007202:Indicators and Reagents