2-(2-(Pyren-1-yl)-1H-benzo[d]imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) and its application for determination of bile acids by HPLC-FLD-MS | |
Xia, Lian ; Wu, Chuanxiang ; Sun, Zhiwei ; You, Jinmao | |
刊名 | ANALYTICAL METHODS
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2014 | |
英文摘要 | A method of high performance liquid chromatography-fluorescence detection-mass spectrometry identification (HPLC-FLD-MS) coupled with pre-column derivatization to determine bile acids (BAs) from bio-sample has been developed here. The labeling reagent of 2-(2-(pyren-1-yl)-1H-benzo[d] imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) contains six benzene rings and two weak basic nitrogens in the structure, resulting in a higher degree of conjugation and perfect ionization efficiency. The PBITS could easily and quickly label BAs at the optimized derivatization conditions and the labeling yield was close to 100%. Separation of the derivatized BAs exhibited a good baseline resolution in combination with a gradient elution on a reversed-phase Hypersil BDS C-18 column. Calculated detection limits for HPLC-FLD, at a signal-to-noise ratio of 3, were 10.09-16.33 fmol. Excellent linear responses were observed with correlation coefficients >0.9995. The mean inter-day precision for all standards was <3.63% and the experimental recoveries were 89.9-106.3%. Good compositional data were obtained from the analysis of the extracted BAs from pig bile sample. Therefore, the facile PBITS derivatization coupled with HPLC-FLD-MS analysis allowed the development of a highly sensitive method for the quantization of trace levels of BAs from biological samples.; A method of high performance liquid chromatography-fluorescence detection-mass spectrometry identification (HPLC-FLD-MS) coupled with pre-column derivatization to determine bile acids (BAs) from bio-sample has been developed here. The labeling reagent of 2-(2-(pyren-1-yl)-1H-benzo[d] imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) contains six benzene rings and two weak basic nitrogens in the structure, resulting in a higher degree of conjugation and perfect ionization efficiency. The PBITS could easily and quickly label BAs at the optimized derivatization conditions and the labeling yield was close to 100%. Separation of the derivatized BAs exhibited a good baseline resolution in combination with a gradient elution on a reversed-phase Hypersil BDS C-18 column. Calculated detection limits for HPLC-FLD, at a signal-to-noise ratio of 3, were 10.09-16.33 fmol. Excellent linear responses were observed with correlation coefficients >0.9995. The mean inter-day precision for all standards was <3.63% and the experimental recoveries were 89.9-106.3%. Good compositional data were obtained from the analysis of the extracted BAs from pig bile sample. Therefore, the facile PBITS derivatization coupled with HPLC-FLD-MS analysis allowed the development of a highly sensitive method for the quantization of trace levels of BAs from biological samples. |
内容类型 | 期刊论文 |
源URL | [http://ir.nwipb.ac.cn/handle/363003/4284] ![]() |
专题 | 西北高原生物研究所_中国科学院西北高原生物研究所 |
推荐引用方式 GB/T 7714 | Xia, Lian,Wu, Chuanxiang,Sun, Zhiwei,et al. 2-(2-(Pyren-1-yl)-1H-benzo[d]imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) and its application for determination of bile acids by HPLC-FLD-MS[J]. ANALYTICAL METHODS, Xia, L; Wu, CX; Sun, ZW; You, JM.2-(2-(Pyren-1-yl)-1H-benzo[d]imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) and its application for determination of bile acids by HPLC-FLD-MS,ANALYTICAL METHODS,2014,6(4):1135,2014. |
APA | Xia, Lian,Wu, Chuanxiang,Sun, Zhiwei,&You, Jinmao.(2014).2-(2-(Pyren-1-yl)-1H-benzo[d]imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) and its application for determination of bile acids by HPLC-FLD-MS.ANALYTICAL METHODS. |
MLA | Xia, Lian,et al."2-(2-(Pyren-1-yl)-1H-benzo[d]imidazol-1-yl)-ethyl-4-methyl benzenesulfonate (PBITS) and its application for determination of bile acids by HPLC-FLD-MS".ANALYTICAL METHODS (2014). |
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