Liu Haolong, Fan Miaoxuan, Fu Xintong, Chen Yougen, Ye Min, Guo Hongzhu
School of Pharmaceutical Sciences, Peking University, 38 Xueyuan Road, Beijing 100191, China.
NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine), Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing Institute for Drug Control, 25 Kexueyuan Road, Beijing 102206, China.
J Chromatogr Sci. 2020 Jun 5;58(6):542-548. doi: 10.1093/chromsci/bmaa017.
The excreta of Trogopterus xanthipes (also called Wulingzhi in Chinese, WLZ) is a well-known traditional Chinese medicine used for the treatment of irregular menstruation in clinic. Few reports are available on the chemical profiling of WLZ. In this work, qualitative and quantitative analyses of endogenous prostaglandin and hormones in WLZ were performed using UHPLC-orbitrap-MSn. In total, 48 compounds were identified in urine of T. xanthipes. Furthermore, the contents of four target compounds were simultaneously quantitated in 20 batches of samples by UPLC-MS/MS. The quantitative method showed a good linear correlation (R > 0.995) in a wide range for each compound. The method had a high sensitivity with LOD (0.5-1.0 ng/mL) and LOQ (1.0-2.5 ng/mL). The intra- and inter-day precisions were < 9.17 (RSD %), and repeatability and stability were < 6.14 (RSD %). The recovery of the analytes varied between 85.8% and 97.3% at three different concentrations. The present integrated qualitative and quantitative assessment of WLZ provides an evaluation strategy to assess the constituent in traditional Chinese medicine.
鼯鼠粪(中药名为五灵脂,WLZ)是临床上用于治疗月经不调的一种著名的传统中药。关于五灵脂的化学图谱分析的报道较少。在这项工作中,使用超高效液相色谱-轨道阱-质谱联用仪(UHPLC-orbitrap-MSn)对五灵脂中的内源性前列腺素和激素进行了定性和定量分析。总共在鼯鼠尿液中鉴定出48种化合物。此外,通过超高效液相色谱-串联质谱(UPLC-MS/MS)同时对20批样品中的四种目标化合物进行了定量分析。定量方法对每种化合物在很宽的范围内均显示出良好的线性相关性(R>0.995)。该方法具有高灵敏度,检测限(LOD)为0.5 - 1.0 ng/mL,定量限(LOQ)为1.0 - 2.5 ng/mL。日内和日间精密度均<9.17%(相对标准偏差,RSD%),重复性和稳定性均<6.14%(RSD%)。在三种不同浓度下,分析物的回收率在85.8%至97.3%之间。目前对五灵脂进行的综合定性和定量评估提供了一种评估中药成分的策略。