| Traditional Chinese medicine and its products have been treasures of our country for thousands of years.The demand of traditional Chinese medicine is increasing with the advancement of technology and the development of society.The subsequent problem is how to control its quality.As we all know,the composition of traditional Chinese medicine is extremely complex.There is much interference impurities and the content of some active ingredients is low,which brings huge problems and challenges to the quality analysis of traditional Chinese medicine.A reasonable sample preparation method become the key which solve the problem.Traditional sample preparation methods are time-consuming and labor-intensive and need large amounts of organic solvents.Therefore,it is very important to explore simple,efficient and green sample preparation methods for the extraction and analysis of active ingredients of traditional Chinese medicine.In this paper,traditional Chinese medicine Rheum palmatum L.and Cnidium monnieri(L.)Cuss.were used as sample matrix.The matrix solid phase dispersion extraction was improved and innovated.Then,high-performance liquid chromatography with a diode array detector was used for the determination of target analytes.It is mainly divided into the following two parts.(1)The ionic liquid-immobilized NaY zeolite was prepared by means of impregnation approach and used as the dispersant of matrix solid phase dispersion for the extraction of aloe-emodin,emodin,chrysophanol and phy scion in Rheum palmatum L..High performance liquid chromatography coupled with diode-array detection was used for the separation and determination of target analytes.The ionic liquid-immobilized NaY zeolite was further characterized by SEM,FT-IR,TA,XRD and BET.The experimental parameters,such as type and content of ionic liquid,mass ratio of sample to dispersant,type of washing solvent,and type and volume of elution solvent,were optimized.The results revealed that the prepared ionic liquid-immobilized NaY zeolite presents suitable properties and can be used as the dispersant of matrix solid phase dispersion for the extraction of anthraquinones.Good linearities(r?0.9995)were obtained in the range of analyte concentration investigated.The recoveries were 73.3%-98.2%with the relative standard deviations lower than 6.0%.Compared with ultrasound-assisted extraction and heat reflux extraction,the present method requires less sample,organic solvent and extraction time.The present method can be applied to the determination of anthraquinones from medicinal plant.(2)A dynamic temperature-controlled matrix solid-phase dispersion coupled with high performance liquid chromatography method was established for the determination of three coumarin compounds,such as bergamot lactone,imperatorin and osthole in the Cnidium mmonnieri(L.)Cuss..In present study,the peristaltic pump was used to control the flow rate of the eluent and the heating pad was used to control the temperature of the extraction system The dynamic extraction was combined with the temperature control to further improve the extraction efficiency of the matrix solid phase dispersion.The experimental parameters,such as type of dispersant,mass ratio of sample to dispersant,type of washing solvent,type and volume of elution solvent,preheating time and heating temperature were optimized.The experimental results showed that each target analyte had a good linear relationship(r?0.9995)within the investigated concentration range.The spiked recovery was 73.9%-95.7%,and the relative standard deviation was lower than 6.0%.Compared with the standard method of the Chinese Pharmacopoeia,the present method consumed the less samples,reagents and extraction time,though there was no significant difference in extraction yield.Compared with the traditional heat reflux extraction,the present method had the high extraction yield when the less sample,solvent and time was consumed.Therefore,the present method can be widely applied to the extraction and detection of coumarin compounds in Chinese medicinal materials. |
PDF Full Text Request