Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001, China.
Anal Bioanal Chem. 2010 Apr;396(7):2657-66. doi: 10.1007/s00216-010-3467-4. Epub 2010 Feb 6.
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).
2-(5-苯并吖啶基)乙基对甲苯磺酸盐（BAETS）是一种双敏探针，它在 K2CO3 催化剂存在下与胆汁酸在二甲亚砜（DMSO）溶剂中反应，生成 BAETS-胆汁酸衍生物。衍生物在 270nm 处表现出强烈的荧光（FL）激发最大值和 510nm 处的发射最大值。使用 APCI-MS 的 MS 分析表明，衍生物具有出色的 APCI-MS 离解能力，水相乙腈中的离解百分比变化范围为 0 至 88.83%，水相甲醇中的离解百分比变化范围为 0 至 89.15%。m/z [M + H]（+）的碰撞诱导解离谱包含特定的碎片离子，m/z 分别为 [M + H-H2O]（+）、[M + H-2H2O]（+）、[M + H-3H2O]（+）、347.3 和 290.1。使用水相乙腈作为流动相时，BAETS-胆汁酸衍生物的 LC 分离重复性良好。荧光检测（FL）下，在 6.6nmol·mL-1 水平时，保留时间和峰面积的相对标准偏差（RSD）分别为 0.045%至 0.072%和 2.16%至 2.73%。观察到良好的线性响应，回归系数>0.9995。FL 检测限（S/N = 3）在 18.0-36.1fmol 范围内。在线 APCI-MS 检测限在 500-790fmol 范围内（信噪比为 3）。
