Wang Anqi, Li Zheng, Wang Jinghui, Liu Haolong, Fu Xintong, Chen Yougen, Guo Hongzhu
School of Pharmaceutical Sciences, Peking University, Beijing, 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, Beijing, China.
Biomed Chromatogr. 2023 Nov;37(11):e5726. doi: 10.1002/bmc.5726. Epub 2023 Aug 31.
The excreta of Trogopterus xanthipes ("Wulingzhi" in Chinese, WLZ) is a well-known traditional Chinese medicine. It has been used for centuries to treat amenorrhea, menstruation and postpartum abdominal pain. However, a systematic quality study on WLZ chemical markers has yet to be conducted. This study aimed to establish an ultra-high-performance liquid chromatography coupled with a hybrid quadruple extraction Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap-HRMS) method for the simultaneous quantitative determination of 20 compounds in 53 batches of WLZ; the method rapidly and sensitively determined the 20 plant- or animal-derived compounds. Firstly, the proposed approach was validated to satisfy the method's linearity, detection limits, precision, repeatability, stability and accuracy. Subsequently, multivariate analysis was used to identify correlations between the samples and feed, processing and regions. Finally, this method was used to further identify chemical markers for quality control in combination with chemometrics. This is the first report on pinusolide, betaine, hippuric acid, 4-oxorentinoic acid, 15-methoxypinusolidic acid and 4-oxoisotrentinoin in WLZ; the quality of WLZ became homogeneous after processing with vinegar (V-WLZ). Moreover, we screened for potential component markers, including uridine, allantoin, amentoflavone, hippuric acid, 3,4-dihydroxybenzoic acid, pinusolide, quercetin and kaempferol. These results were practical and efficient for the chemical clarification of WLZ and V-WLZ.
五灵脂是一种著名的传统中药。几个世纪以来，它一直被用于治疗闭经、月经不调和产后腹痛。然而，尚未对五灵脂的化学标志物进行系统的质量研究。本研究旨在建立一种超高效液相色谱-混合四极杆-轨道阱高分辨率质谱联用（UHPLC-Q-Orbitrap-HRMS）方法，用于同时定量测定53批次五灵脂中的20种化合物；该方法能快速、灵敏地测定这20种植物或动物来源的化合物。首先，对所提出的方法进行验证，以满足方法的线性、检测限、精密度、重复性、稳定性和准确性。随后，采用多变量分析来确定样品与产地、加工方式和产地之间的相关性。最后，结合化学计量学，使用该方法进一步鉴定质量控制的化学标志物。这是首次报道五灵脂中含有松脂醇二乙酸酯、甜菜碱、马尿酸、4-氧代视黄酸、15-甲氧基松脂醇二乙酸酯和4-氧代异视黄酸；醋制五灵脂（V-WLZ）加工后，五灵脂的质量变得均匀。此外，我们筛选了潜在的成分标志物，包括尿苷、尿囊素、穗花杉双黄酮、马尿酸、3,4-二羟基苯甲酸、松脂醇二乙酸酯、槲皮素和山奈酚。这些结果对于五灵脂和醋制五灵脂的化学表征具有实际意义且高效。
