Song Yue, He Qing, Li Ping, Cheng Yi-Yu
Department of Chinese Medicine Science & Engineering, Zhejiang University, Hangzhou, People's Republic of China.
J Sep Sci. 2008 Jan;31(1):64-70. doi: 10.1002/jssc.200700259.
In this study, a rapid and reliable assay has been developed for quantification of pinane monoterpene glycosides in cortex Moutan; it is based on capillary high performance liquid chromatography coupled with electrospray ionization mass spectrometry (capillary HPLC-ESI MS). This method utilizes capillary HPLC for the separation of seven pinane monoterpene glycosides in a methanol extract of the botanical sample followed by negative ion electrospray ionization and single ion monitoring (SIM). The compounds of interest in the sample were unambiguously identified on the basis of information about retention time and quasi-molecular ions (M-H) or adduct ions (M+HCOO). Validation parameters of the method were established. The linearity range was 1.01-105.5 microg/mL with the square of correlation coefficients lying in the range of 0.9965-0.9997, limits of detection were on the fmol level, the average recoveries varied between 91.8 and 101.0%, and good precision values (RSD, 1.2-4.91%) for peak area were obtained. After validation, the applicability of the method for determination of these pinane monoterpene glycosides in cortex Moutan has been demonstrated.
本研究建立了一种快速可靠的测定牡丹皮中蒎烷单萜苷含量的方法；该方法基于毛细管高效液相色谱-电喷雾电离质谱联用技术（毛细管HPLC-ESI MS）。该方法利用毛细管HPLC对植物样品甲醇提取物中的7种蒎烷单萜苷进行分离，然后进行负离子电喷雾电离和单离子监测（SIM）。根据保留时间和准分子离子（M-H）或加合离子（M+HCOO）的信息，明确鉴定了样品中的目标化合物。建立了该方法的验证参数。线性范围为1.01-105.5 microg/mL，相关系数平方在0.9965-0.9997之间，检测限在飞摩尔水平，平均回收率在91.8%至101.0%之间，峰面积的精密度良好（RSD，1.2-4.91%）。经过验证，证明了该方法在测定牡丹皮中这些蒎烷单萜苷方面的适用性。
