Wang Yinan, Han Fei, Song Aihua, Wang Miao, Zhao Min, Zhao Chunjie
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning Province, China.
School of Life Science and Biopharmaceutics, Shenyang Pharmaceutical University, Shenyang, Liaoning Province, China.
J Sep Sci. 2016 Nov;39(22):4325-4334. doi: 10.1002/jssc.201600851. Epub 2016 Oct 12.
Cortex Fraxini is an important traditional Chinese medicine. In this work, a rapid and reliable homogenate extraction method was applied for the fast extraction for Cortex Fraxini, and the method was optimized by response surface methodology. Ultra high performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry and gas chromatography with mass spectrometry were established for the separation and characterization of the constituents of Cortex Fraxini. Liquid chromatography separation was conducted on a C column (150 mm × 2.1 mm, 1.8 μm), and gas chromatography separation was performed on a capillary with a 5% phenyl-methylpolysiloxane stationary phase (30 m × 0.25 mm × 0.25 mm) by injection of silylated samples. According to the results, 33 chemical compounds were characterized by liquid chromatography with mass spectrometry, and 11 chemical compounds were characterized by gas chromatography with mass spectrometry, and coumarins were the major components characterized by both gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. The proposed homogenate extraction was an efficient and rapid method, and coumarins, phenylethanoid glycosides, iridoid glycosides, phenylpropanoids, and lignans were the main constituents of Cortex Fraxini. This work laid the foundation for further study of Cortex Fraxini and will be helpful for the rapid extraction and characterization of ingredients in other traditional Chinese medicines.
秦皮是一种重要的传统中药。在本研究中,采用快速可靠的匀浆提取法对秦皮进行快速提取,并通过响应面法对该方法进行优化。建立了超高效液相色谱结合傅里叶变换离子回旋共振质谱以及气相色谱-质谱联用方法,用于秦皮成分的分离与表征。液相色谱分离在C柱(150 mm×2.1 mm,1.8μm)上进行,气相色谱分离采用5%苯基-甲基聚硅氧烷固定相的毛细管柱(30 m×0.25 mm×0.25 mm),进样硅烷化样品。结果表明,液相色谱-质谱联用鉴定出33种化合物,气相色谱-质谱联用鉴定出11种化合物,香豆素类是气相色谱-质谱联用和液相色谱-质谱联用鉴定出的主要成分。所提出的匀浆提取法是一种高效快速的方法,香豆素类、苯乙醇苷类、环烯醚萜苷类、苯丙素类和木脂素类是秦皮的主要成分。本研究为秦皮的进一步研究奠定了基础,有助于其他传统中药成分的快速提取与表征。