| Purpose:By applying COFs to the pretreatment materials ofα-asarone,β-asarone and methyl isoeugenol in complex Chinese medicine extracts and biological samples,we can enrich the pretreatment materials in Chinese medicine samples and provide new exploration for the research and development of Chinese medicine pretreatment methods,Methods:1.The active ingredients in Acorous Tatarinowii Rhizoma purchased from Tong Ren Tang Pharmacy were screened for active ingredients by gas chromatography-mass spectrometry(GC-MS)technique,and determine the contents ofα-asarone andβ-asarone.Combined with the determination of moisture,ash and leachate,the quality determination of the samples of Acorous Tatarinowii Rhizoma were comprehensively analyzed.2.Fe3O4 magnetic nanoparticles were synthesized by hydrothermal method,and then1,3,5-trihydroxyresorcinol(Tp)and benzidine(BD)were used as ligands to generate Tp BD-COF@Fe3O4 with core-shell structure and used for the separation and extractionα-asarone andβ-asarone in pharmaceutical solutions based on the principle of monomer mediation;the prepared composites were characterized by TEM,FT-IR and other characterization methods and the adsorption conditions were optimized.3.The composites of MS@Tp BD were obtained by hydrothermal method and used as materials for syringe-solid phase extraction,then used for the treatment ofα-asarone,β-asarone and methyl isoeugenol in rat serum.Combined with GC-MS to detect the extracted efficiency;the synthesized composites were characterized by SEM and FT-IR,the adsorption conditions were also optimized.Results:1.The total volatile oil content of Acorous Tatarinowii Rhizoma was 2.5%,the extract content was 14.4%,the moisture content was 6.7%and the total ash content was 9.5%,all of them could meet the quality requirements of the 2020 edition of the Chinese Pharmacopoeia.The GC-MS total ion flow map of the root drama showed that the total volatile oil extract of Acorous Tatarinowii Rhizoma contained 50 compounds;the contents ofα-asarone andβ-asarone were 4.64 mg/g and 15.66 mg/g,respectively.2.Tp BD-Fe3O4 was successfully synthesized based on SEM and FT-IR characterization;the adsorption recoveries ofα-asarone andβ-asarone in the combined decoction of Acorous Tatarinowii Rhizoma and Polygalae Radix were above 90%by MSPE-HPLC with low limits of detection(<0.044μg/m L)and quantification(<0.15μg/m L).3.It was demonstrated that MS@Tp BD had been successfully synthesized based on SEM and FT-IR;the adsorption recoveries ofα-asarone,β-asarone and methyl isoeugenol in rat serum samples by SPE-GC-MS were higher than 90%,with the detection limit of 0.015μg/m L and the quantification limit of 0.60μg/m L.Conclusion:1.The MSPE-HPLC method constructed by combining Tp BD-Fe3O4 as the adsorbent of MSPE and combined with HPLC which can be used for the complex Chinese medicine extract samples withα-asarone andβ-asarone and successfully achieved the good separation of the asarone components.The MSPE-HPLC method was demonstrated to be feasible as a pretreatment method for complex samples containingα-asarone andβ-asarone.2.The SPE-GC-MS constructed by combining MS@Tp BD as the sorbent of the syringe-solid phase extraction method with GC-MS which was used for the separation ofα-asarone,β-asarone and methyl isoeugenol in rat serum samples.That has pioneered a new strategy for the pretreatment method of blood-incorporating components of Acorous Tatarinowii Rhizoma in biological samples. |