HPLC-MS/MS法测定兔血浆中黄芪甲苷的含量

目的 建立兔含药血浆中黄芪甲苷含量快速测定的新方法.方法 固相萃取法富集血浆中的黄芪甲苷;Agilent SB-C18反相色谱进行分离;采用离子阱质谱多级反应模式,以m/z 807.5→627.1为选择离子对,内标法测定含量.结果 血浆中黄芪甲苷的检测限为0.1ng/mL,线性范围为0.5～50.0μg/mL,平均方法回收率在96.3%～104.7%范围内.结论 该方法具有灵敏度高、稳定性好和快速的特点,符合生物样品的分析要求,有望用于黄芪甲苷的药代动力学研究.     

HPLC-MS法测定兔血浆和组织中丹参素异丙酯的含量

目的 建立兔血浆及组织中β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯(丹参素异丙酯)的高效液相色谱-电喷雾-离子阱质谱(LC-ESI-MSn)测定新方法.方法 采取液液萃取法处理血浆及组织样品,以4-羟基苯甲酸甲酯为内标,LC-ESI-MSn多级反应模式测定血浆及组织中丹参素异丙酯的含量.结果 丹参素异丙酯在血浆、心、肝、脾、肺、肾和脑中的检出限分别为:0.54、1.08、1.20、1.62、2.15、1.12、1.36ng/mL,线性范围分别为:0.20～400、0.10～200、0.01～100、0.02～400、0.20～800、0.01～100和0.05～100μg/mL,日内、日间精密度的相对标准偏差均小于10%,方法平均回收率在89.5%～107.4%范围内.结论 该分析方法灵敏度高、专属性好,为丹参素异丙酯的非临床和临床药代动力学研究提供一种方法学参考.     

CO_2超临界流体萃取丹参中的有效成分

目的　建立CO2 超临界流体萃取丹参中有效成分的方法 ,并用高效液相 质谱法进行产物分析。方法　以 95 0mL·L-1乙醇为夹带剂 ,在 2 0MPa、4 5℃条件下 ,萃取丹参药材 1h后 ,再在 30MPa、6 5℃条件下 ,以 10 0mL·L-1的乙醇为夹带剂萃取 2h ,并将超临界萃取法与回流提取法、超声提取法进行了比较。结果　超临界萃取法萃取的成分最多 ,萃取效率也高于其他两种方法。结论　超临界萃取法提取丹参中有效成分耗时少、准确、效率高且提取完全。     

Rapid analysis of components in Rhizoma Anemarrhenae by HPLC-DAD-MS and HPLC-DAD-TOFMS

A global quality control method based on high performance liquid chromatography (HPLC) coupled with diode array detection (DAD), single quadrupole mass spectrometry (MS) and time-of-flight mass spectrometry (TOFMS) was developed for simultaneous determination of seven major components (mangiferin, neomangiferin, timosaponin E1, timosaponin E, timosaponin BⅡ, timosaponin BⅢ, and timosaponin AⅢ) and identification of most components in extracts of Rhizoma Anemarrhenae (RA). HPLC analysis was performed on an Agilent SB-C18 column (4.6 mm×150 mm, 5 μm) by gradient elution using acetonitrile and water-acetic acid(100∶0.05, v/v) as the mobile phase. Seven major components in RA were successfully separated. This quantitative method was fully validated in respect of the following performance criteria: linearity, precision, repeatability, stability, accuracy, limits of detection (LOD) and quantification (LOQ). A formula database of known compounds in RA was established, against which, most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS. This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China. This global quality control method, which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components, is suitable for routine quantification and comprehensive quality control of RA.