Development Of The New Methods For The Analysis Of Anthraquinones And Alkaloids In Some Edible And Medicinal Substances

Homology of medicine and food has a long history in China.However,the application process of edible and medicinal substances is also accompanied with poisoning events.Therefore,the researching and developing of new technology for the analysis of endogenous hazardous components of edible and medicinal substances will provide effective technical reference for the formulation or revision of food safety supervision standards of China,reduce the occurrence of food safety accidents,and effectively promote the healthy and rapid development of related industries.In this paper,new methods for the analysis of anthraquinones and alkaloids in edible and medicinal materials(Polygonum multiflorum,Cassiae Semen and Aconiti Laterais Radix Praeprate)was established with ultra-high performance liquid chromatography(UHPLC).The developed methods have been applied to the determination of real samples with satisfactory results.The main research results are as follows:1.A rapid and effective ultra-high performance liquid chromatography(UHPLC)method was developed for the determination of five anthraquinones(emodin,physcion,aloe-emodin,rhein,and chrysophanol)in Polygonum multiflorum.The target compounds were ultrasonically extracted with 70%methanol,followed by dispersive solid-phase extraction(d-SPE)with HC-C18 and desorption with acetonitrile.The five anthraquinones were separated on an ACQUITY UPLC HSS T3column(2.1mm×100 mm,1.8μm)and detected by a photodiode array detector(PDA)at 254 nm.Under the optimized conditions,linear relationships were achieved in the range of 0.3～100 mg/L for emodin,0.3～40 mg/L for physcion,0.1～20 mg/L for aloe-emodin,and 0.05～20 mg/L for rhein and chrysophanol.The limits of detection of the five analytes ranged from 0.01 to 0.08 mg/L,and the recoveries were within the range of 82.8～118.4%with an RSD(n=6)of 1.0～10.3%.The intra-day and inter-day precision(n=5)of the five targets were in the range of 1.0～1.8%and 3.0～3.1%,respectively.Furthermore,this method was applied to analyses of Polygonum multiflorum samples collected from different regions in China with satisfactory results.2.A novel,efficient and effective UHPLC method was developed for the simultaneous determination of seven anthraquinones(aurantio-obtusin,aloe-emodin,rhein,obtusin,emodin,chrysophanol and physcion)in Cassiae Semen.The method firstly applied natural deep eutectic solvent(NADES)with designable physiochemical properties and low toxicity to the extraction of the seven anthraquinones from Cassiae Semen.New NADESs were designed by menthol,choline chloride,D-glucose as hydrogen bond acceptors,with 7 different acids and appropriate water as hydrogen bond donors.Among obtained NADESs,the highest extraction efficiency was demonstrated by a liquid consisting of D-glucose,lactic acid and water with a molar ratio of 1:5:4.The seven anthraquinones were separated on an ACQUITY UPLC(?)BEH C18 column(2.1 mm×100 mm,1.8μm)and detected within 12 minutes by a photodiode array detector(PDA)at 254 and 284 nm.For the proposed method,the parameters affecting the extraction efficiency of seven anthraquinones were optimized,and the limits of detection and quantitation were from 1.00 to 7.26μg/L and 3.29 to 24.22μg/L,respectively.And Cassiae Semen sample based recoveries were ranged from 81.1%to 113.8%with the RSD(n=6)of1.4%to 10.1%.The developed method was successfully applied to analyze the anthraquinones in Cassiae Semen samples collected from different regions in China.3.A new method was established for the determination of three diester alkaloids(mesaconitine,hypaconitine and aconitine)in Aconiti Laterais Radix Praeprate by ultra-high performance liquid chromatography(UHPLC).The three diester alkaloids were separated by a Shim-pack XR-ODSⅢcolumn(2 mm×75 mm,1.6μm)and detected by a photodiode array detector(PDA)at 230 nm.The sample was firstly soaked with ammonia reagent and then ultrasonically extracted with ether,the extraction conditions were optimized.Under the optimized conditions,linear relationships were achieved in the range of 2～100 mg/L for mesaconitine and aconitine,2～180 mg/L for hypaconitine,(R~2≥0.9976).The limits of detection and quantitation were 0.27～0.49 mg/L and 0.91～1.65 mg/L,respectively.The recoveries were 70.2～105.2%with relative standard deviations(n=6)of 1.4～5.6%.