Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang, P. R. China.
J Sep Sci. 2010 Mar;33(4-5):545-57. doi: 10.1002/jssc.200900704.
A novel method, HPLC-MS/MS was developed to qualitatively identify and quantitatively determine the 28 components including 19 diterpenoids, 6 phenolic acids and 3 flavonoids in Isodon rubescens, an important traditional Chinese medicine. The separation was performed on a C(18) column with linear gradient elution with 0.1% aqueous formic acid/methanol containing 0.1% formic acid at a flow rate of 0.7 mL/min. The identification and quantification of those analytes were achieved on a hybrid quadrupole linear ion trap mass spectrometer. Multiple-reaction monitoring scanning was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. Full validation of the method was carried out (linearity, precision, accuracy, LOD and LOQ). The results indicated that the method was simple, rapid, specific and reliable. The proposed method was successfully applied for the qualitative and quantitative analysis of 28 chemical compositions in 21 batches of natural and cultured I. rubescens samples from different sources which had great variation on the contents. The results demonstrated that the method was useful for standardization and differentiation of large numbers of similar samples.
建立了一种高效液相色谱-串联质谱法（HPLC-MS/MS），用于定性分析和定量测定毛萼香茶菜中 28 种化学成分，包括 19 种二萜、6 种酚酸和 3 种黄酮类化合物。采用 C18 柱，以 0.1%甲酸/甲醇（含 0.1%甲酸）为流动相进行线性梯度洗脱，流速为 0.7 mL/min。在混合四极杆线性离子阱质谱仪上进行鉴定和定量分析。采用正负切换电喷雾离子源极性的多反应监测扫描方式，在单次运行中对这些分析物进行定量分析。对该方法进行了全面验证（线性、精密度、准确度、检出限和定量限）。结果表明，该方法简单、快速、特异性好、可靠。该方法成功应用于 21 批不同来源的天然和栽培毛萼香茶菜样品中 28 种化学成分的定性和定量分析，这些样品的含量存在较大差异。结果表明，该方法对于大量类似样品的标准化和区分具有重要意义。
