Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Wuhan University), Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan, China.
J Sep Sci. 2012 Jul;35(13):1644-50. doi: 10.1002/jssc.201200173.
Bavachin and isobavachalcone are the isomeric compounds in the fructus Psoraleae. The ion trap mass spectrometric fragmentation pathways of the bavachin and isobavachalcone in negative ion mode were elucidated for the identification. A novel method for determination of isomeric bavachin and isobavachalcone has been developed by capillary electrophoresis coupled with mass spectrometric detection. The effects of several factors such as concentration, pH of ammonium acetate buffer, separation voltage, composition and flow rate of the sheath liquid were investigated. Under optimal conditions, the linear concentration range for bavachin and isobavachalcone were 0.8-100 μg/mL with the correlation coefficient of 0.996 and 0.995, respectively. Relative standard deviations of migration time and peak areas were lower than 5%. The limits of detection (signal/noise = 3) were 60 ng/mL. The proposed method can be successfully applied to the determination of bavachin and isobavachalcone in the fructus Psoraleae and six fructus Psoraleae-containing preparations.
补骨脂素和异补骨脂素是补骨脂中的同分异构体化合物。采用离子阱质谱法,在负离子模式下,对补骨脂素和异补骨脂素的碎裂途径进行了阐述,以进行鉴定。建立了一种新的毛细管电泳-质谱联用测定同分异构体补骨脂素和异补骨脂素的方法。考察了浓度、乙酸铵缓冲液 pH 值、分离电压、鞘液组成和流速等因素的影响。在最佳条件下,补骨脂素和异补骨脂素的线性浓度范围分别为 0.8-100μg/mL,相关系数分别为 0.996 和 0.995。迁移时间和峰面积的相对标准偏差均低于 5%。检测限(信噪比=3)为 60ng/mL。该方法可成功应用于补骨脂及其 6 种含补骨脂制剂中补骨脂素和异补骨脂素的测定。