Application Of New Sample Pretreatment Technique In Analysis Of Active Compounds In Traditional Chinese Medicine

Sample pretreatment which greatly affects the accuracy and sensitivity of the analysis results,plays a vital role in the quality control of traditional Chinese medicines and the determination of active ingredients.Matrix solid phase dispersion(MSPD)extraction is a new sample pretreatment technique with the advantages of simple,fast,economical and environmentally friendly.It can be used for the extraction of active ingredients from traditional Chinese medicines.Therefore,in order to improve the extraction efficiency of active ingredients from traditional Chinese medicines and reduce the consumption of materials,this study developed suitable MSPD adsorbent materials,combined appropriate assistive technologies and miniaturized MSPD.In addition,the established methods have been applied to complex traditional Chinese medicine samples.The main research contents are as follows:1.A green ionic-liquid based vortex-synchronized matrix solid-phase dispersion(VS-MSPD)combined with HPLC method was developed to determine four anthraquinones(aurantio-obtusin,chrysoobtusin,obtusifolin and emodin)in Cassiae Semen samples.Crab shell powder(CSP)from abandoned crab shells was developed as the adsorbent.The pivotal factors affecting the extraction efficiency of VS-MSPD were investigated and optimized by the single-factor experiment,including the type of adsorbent,sample/adsorbent ratio,grinding time,vortex time,the type and concentration of ionic liquids.As the results shown,the established method had satisfying linearities(R>0.999),good repeatability(RSD≤4.60%),desirable stability(RSD≤3.15%)and high recovery(91.30%-106.40%).In addition,the method was successfully applied to sample preparation and determination of anthraquinones in five batches of Cassiae Semen samples.Moreover,the adsorption effect of CSP on different types of compounds was discussed,which provided a feasible direction forthe application of CSP as an adsorbent in the sample pretreatment of active ingredients of traditional Chinese medicines.2.A deep eutectic solvent(DES)based ultrasonic-synchronized matrix solid-phase dispersion(US-MSPD)combined with HPLC method was developed to determine four flavonoids(baicalin,wogonoside,baicalein and wogonin)in Scutellaria Radix.Meanwhile,molecular sieve ZSM-5 was used as the adsorbent.The pivotal parameters affecting the extraction efficiency of US-MSPD were studied and optimized by the single-factor experiment and the response surface methodology based on Box-Benhnken design.Besides,the design space is constructed and verified to confirm the operating space.The results showed that the established method had good linearities(R>0.999),desirable repeatability(RSD≤2.24%),excellent stability(RSD≤2.87%)and satisfactory recovery(95.90%-102.31%).What’s more,the method was successfully applied to sample preparation and quantitative analysis of flavonoids in nine batches of Scutellaria Radix samples.3.A molecular sieve(SBA-3)-based pipette-tip miniaturized matrix solid-phase dispersion(PT-MMSPD)microextraction combined with HPLC method was developed to simultaneously determine lignans(honokiol and magnolol)and terpenes(costunlide and dehydrocostus lactone)in a complex Chinese Patent Medicines named Muxiang Shunqi pills.A tiny amount of sample and adsorbent consumption(3 mg of sample and 6 mg of SBA-3)was adopt.The main parameters affecting the extraction efficiency of PT-MMSPD microextraction were explored and optimized by the single-factor experiment and the response surface methodology based on Box-Benhnken design.It can be seen that the developed method had a excellent linearities(R>0.999),good stability(RSD≤3.02%),satisfactory repeatability(RSD≤4.93%)and desirable recovery(95.79%-102.81%).Besides,the established method was successfully applied to sample preparation and determination of lignans and terpenes in three batches of Muxiang Shunqi pills.