ABSTRACT
Objective:To screen qualitative preparation quality markers of Yuliantang， in order to provide data support for the selection of indicator components， and establish the direct connection between indicator components and efficacy （Xiehuo Zhitong） for achieving the quantity-effect combination. Method:The stability of preparation process of Yuliantang lyophilized powder was investigated by HPLC fingerprint technology， then， the components in Yuliantang lyophilized powder were identified by UHPLC-LTQ-Orbitrap-MS. By referring to the relevant literature， the pharmacological activities of these identified compounds were compared with the pharmacological effects corresponding to the efficacy of Yuliantang， and the composition of the qualitative preparation quality markers of Yuliantang lyophilized powder was determined. Result:The similarities between HPLC fingerprint of 10 batches of Yuliantang lyophilized powder and the control fingerprint were >0.9， indicating that the preparation process was stable and feasible. A total of 29 components were identified from Yuliantang， of which 23 alkaloids， 3 phenylpropanoids， 2 sesquiterpenoids and 1 limonoid， and there were 15 ingredients of<italic> </italic>Coptidis Rhizoma， 12 ingredients of<italic> </italic>Euodiae Fructus， and 2 ingredients of<italic> </italic>Aucklandiae Radix. The composition of the qualitative preparation quality markers of Yuliantang was initially determined as magnoflorine or 10-hydroxy-2，3，9-trimethoxyberberine， phellodendrine， menisperine， thalifendine， groenlandicine， dehydroevodiamine， coptisine， jatrorrhizine， columbamine， methylcoptisine， berberine， epiberberine， palmatine， evodiamine， rutaecarpine， neochlorogenic acid， cryptochlorogenic acid， chlorogenic acid， limonin， costunolide， dehydrocostus lactone. Conclusion:The method for researching and screening the preparation quality markers in Yuliantang lyophilized powder is scientific， reasonable and feasible， it can provide reference for the determination of component indicators in the process research of Yuliantang and qualitative and quantitative indexes in its quality standard.
ABSTRACT
On the basis of the qualitative preparation quality markers of Yulian Decoction, we screened out the quantitative markers and explored a general strategy for analyzing the component migration in Chinese herbal pieces, preparations, and plasma. A method capable of simultaneously determining 28 chemical components in Yulian Decoction was established based on HPLC-MS/MS. This method was used to determine the migrated components in herbal pieces-lyophilized powder preparations-rat plasma after administration of Yulian Decoction. Liquid chromatography was performed under the following conditions: C_(18)-reversed phase chromatographic column(2.1 mm × 100 mm, 1.8 μm); acetonitrile-water(containing 0.1% formic acid) as the mobile phase for gradient elution; the flow rate of 0.2 mL·min~(-1). Electrospray ionization source was adopted for mass spectrometry detection, in which positive and negative ion modes and multiple reaction monitoring were applied. Confirmed by the methodological investigation in linear range, recovery(95.48%-103.4%), precision(RSD, 0.45%-3.8%), stability, and repeatability(RSD, 5.6%-14%), the established method was suitable for the detection and quantification of the components in Yulian Decoction. The results showed that in the lyophilized powder of Yulian Decoction, berberine was greater than 5% in mass fraction, magnoflorine, epiberberine, coptisine, palmatine, and limonin in the range of 1%-5%, and dehydroevodiamine, evodiamine, rutaecarpine, costunolide, and dehydrocostus lactone in the range of 0.002%-1%. Of the 28 components detected in pieces, 27 were found to migrate to the lyophilized powder, and 11 were detected in rat plasma. Fifteen components were preliminarily determined as quantitative preparation quality markers for Yulian Decoction, including berberine, epiberberine, coptisine, palmatine, evodiamine, rutaecarpine, limonin, costunolide, dehydrocostus lactone, magnoflorine, jatrorrhizine, columbamine, groenlandicine, chlorogenic acid, and neochlorogenic acid. In conclusion, the HPLC-MS/MS general strategy was established for analyzing the migration of multiple components in Chinese herbal pieces, preparations, and plasma, which can provide the basis for the screening of quantitative preparation quality markers and multi-index quality control of Yulian Decoction.