胆汁酸的双敏感探针苯并[b]吖啶酮-5-乙基对甲苯磺酸酯荧光检测和APCI-MS 鉴定 | |
付艳艳 ; 宋翠华 ; 秦雪芹 ; 李肖燕 ; 丁明州 ; 孙志伟 ; 夏 莲 ; 索有瑞 ; 李玉林 ; 尤进茂 | |
刊名 | 化学学报
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2010 | |
英文摘要 | 摘要 在Hypersil C18色谱柱上, 利用新型荧光试剂苯并[b]吖啶酮-5-乙基对甲苯磺酸酯(BAETS)作柱前衍生化试剂, 采用梯度洗脱对10 种胆汁酸衍生物进行了优化分离. 在二甲亚砜溶剂中, 以碳酸钾作催化剂, 95 ℃, 45 min 后获得稳定的荧光产物. 衍生物在稳态荧光条件下, 在乙腈和甲醇水溶液中的百分离子化δ 值在0%~88.83%和0%~89.15%范围内. 最大激发和发射波长为λex/λem=272/505 nm. 采用大气压化学电离源(APCI)正离子模式实现了胆汁中胆汁酸的定性定量测定. 线性回归系数均在0.9995 以上, 线性范围宽, 检出限为0.76~1.62 ng/mL。 Abstract On a reversed-phased Hypersil C18 column, 10 bile acid derivatives were separated using 2-(12-oxobenzo[b]acridin-5(12H)-yl)ethyl 4-toluenesulfonate (BAETS) as pre-column derivatization reagentby high-performance liquid chromatography with fluorescence detection and mass spectrum identification inconjunction with a gradient elution. Optimum derivatization, giving the corresponding sensitively fluorescentderivatives, was obtained by the reacting of bile acids with BAETS at 95 ℃ for 30 min in the presenceof basic catalyst potassium carbonate in dimethylsulfoxide solvent. The optimum excitation and emissionwavelengths were at λex/λem 272 nm/505 nm. The percent ionization δ values in aqueous acetonitrile andaqueous methanol were in the range of 0%~88.83% and 0%~89.15% respectively. The identification of bile acid derivatives was obtained on the basis of an atmosphere-pressure chemical ionization source at positivemodel detection. Correlation coefficients are >0.9995, and detection limits at signal-to-noise of 3 are 0.76~1.62 ng/mL for the labeled bile acids. |
内容类型 | 期刊论文 |
源URL | [http://ir.nwipb.ac.cn//handle/363003/2400] ![]() |
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 | 付艳艳,宋翠华,秦雪芹,等. 胆汁酸的双敏感探针苯并[b]吖啶酮-5-乙基对甲苯磺酸酯荧光检测和APCI-MS 鉴定[J]. 化学学报, 付艳艳;宋翠华;秦雪芹;李肖燕;丁明州;孙志伟;夏 莲;索有瑞;李玉林;尤进茂.胆汁酸的双敏感探针苯并[b]吖啶酮-5-乙基对甲苯磺酸酯荧光检测和APCI-MS 鉴定,化学学报,2010,68(7):653-660,2010. |
APA | 付艳艳.,宋翠华.,秦雪芹.,李肖燕.,丁明州.,...&尤进茂.(2010).胆汁酸的双敏感探针苯并[b]吖啶酮-5-乙基对甲苯磺酸酯荧光检测和APCI-MS 鉴定.化学学报. |
MLA | 付艳艳,et al."胆汁酸的双敏感探针苯并[b]吖啶酮-5-乙基对甲苯磺酸酯荧光检测和APCI-MS 鉴定".化学学报 (2010). |
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