Rationales:Ziziphi Spinosae Semen(ZSS)is the dried mature seed of Ziziphus jujuba Mill.var.spinosa(Bunge)Hu ex H.F.Chou,which is the first choice for the treatment of insomnia.Ziziphi Spinosae Semen is rich in flavonoids,alkaloids,saponins and fatty acids.It has the effects of improving sleep,anti-anxiety and anti-depression,and has extremely high medicinal value and market value.The research team conducted content determination on 17 batches of wild Ziziphi Spinosae Semen samples on the market in the early stage,and found that the content of spinosin was lower than the requirement of 0.08%in the 2015 edition of the Chinese Pharmacopoeia.Jujube(Ziziphus Jujuba Mill.)is a wild resource and has no right of ownership.In recent years,the“grabbing”phenomenon of wild Ziziphus jujuba kernels has become more serious.Farmers have picked wild Jujube(Ziziphus Jujuba Mill.)on a large scale from July in the solar calendar since the unsuitable harvest period,dried them,removed the pulp and pit,and sold them all over the country.The difference in the harvest period will bring about changes in the quality of medicinal materials,which is a problem that is very worthy of attention.Therefore,we speculate that“grab the green”may be the main reason for insufficient accumulation of active ingredients,high water content and excessive aflatoxin in wild Ziziphi Spinosae Semen.Therefore,from the perspective of character evaluation and physical and chemical evaluation,this project integrates HPLC and GC-MS technologies to comprehensively analyze the changes in bioaccumulation,color,moisture content,secondary metabolites and fatty acid composition of sauerkraut during different harvest periods.The results of the study will provide a basis for the establishment of a suitable harvest period for Ziziphi Spinosae Semen in the main producing area of Shanxi.Objective:Taking Shanxi Jujube(Ziziphus Jujuba Mill.)kernels as the research object,taking kernel rate,100-seed weight,color,moisture and aflatoxin as evaluation indicators,and integrating HPLC and GC-MS technology for suitable harvesting period and rushing harvest The quality of Ziziphi Spinosae Semen was evaluated.Methods:(1)In July,August,and September in Shanxi in 2019,the growth environment of wild Jujube(Ziziphus Jujuba Mill.)was investigated on site,wild Jujube(Ziziphus Jujuba Mill.)was harvested,dried,soaked,pulped by hand,and dried jujube kernels were dried and crushed to obtain wild ZSS samples.Using Apollo C18column(250 mm×4.6 mm,5μm)chromatographic column,gradient elution was carried out with acetonitrile and 0.1%formic acid water as mobile phases,the column temperature was 30℃,the flow rate was 1.0 m L/min,and the detection wavelength was227.nm and 335 nm,the temperature of the drift tube of the evaporative light scattering detector(ELSD)is 105℃;the air volume flow rate is 2.5 L/min.Using magnoline,spinosin,and jujuboside A as the characteristic peaks respectively,the characteristic map of ZSS produced in Shanxi was established;aconitine,magnolia,vetanin II,spinosin,6’’’-feruylspinosin,jujuboside A,and jujuboside B were the indicator components,and HPLC-UV-ELSD was established to simultaneously determine the content of 7 chemical components in ZSS.(2)Jujube(Ziziphus Jujuba Mill.)was harvested in Yuci District,Shanxi in July,August,September and October 2020,kernel rate and 100-seed weight were calculated;colorimeter was used to determine color value;water content and aflatoxin were determined;The established HPLC-UV-ELSD method was used to determine the content of 7 components in Ziziphi Spinosae Semen at different harvest periods;the Pearson method was used to analyze the correlation between the color value and the content of the7 effective components;the Soxhlet extractor was used The fatty oil of wild Jujube(Ziziphus Jujuba Mill.)was extracted and the oil ratio was calculated.Then,the content of 7 fatty acids in wild Jujube(Ziziphus Jujuba Mill.)in different harvest periods was determined by the SIM mode of GC-MS.Results:(1)This experiment investigated the growth environment of the main producing areas of Jujube(Ziziphus Jujuba Mill.)in Shanxi.The latitudes and longitudes of Linfen Daning,Jinzhong Yuci,and Yuncheng Wenxi were similar.The Yuci producing area had the highest altitude and the lowest temperature during the same harvest period.From a qualitative point of view,a characteristic map of wild Jujube(Ziziphus Jujuba Mill.)produced in Shanxi was established.The results showed that in the HPLC-UV 227nm spectrum,the similarity of the alkaloids of 9 batches of wild Jujube(Ziziphus Jujuba Mill.)samples was 1,and in the HPLC-UV 335 nm spectrum,9 batches of wild Jujube(Ziziphus Jujuba Mill.)The similarity of flavonoids is 0.979~0.991.In the HPLC-ELSD spectrum,the similarity of the saponins in the 9 batches of jujube seed samples was 0.995~0.999,indicating that the alkaloids and saponins contained in each batch of samples were extremely similar,and the results showed that Shanxi produced ZSS.The uniformity is good,which provides a basis for the evaluation of the authenticity of Ziziphi Spinosae Semen produced in Shanxi in the future.From a quantitative point of view,a HPLC-UV-ELSD method was established for the simultaneous determination of 7 active ingredients in Ziziphi Spinosae Semen.The chromatographic conditions were optimized to more effectively separate the isomers of flavonoids and saponins in Ziziphi Spinosae Semen.Body composition.The content determination results show that the factors of origin have a greater impact on the evaluation of the content of alkaloids,saponins and flavonoids in ZSS at different harvest periods.(2)Picking wild Jujube(Ziziphus Jujuba Mill.)from the end of July to mid-October in Yuci,Jinzhong,2020.From the characteristics,color and bioaccumulation(kernel rate,100-seed weight)and chemical composition(moisture,aflatoxin,secondary metabolites and Fatty acid)content comprehensively evaluated the quality change law of ZSS during suitable harvest period and early harvest period.From the perspective of traits and color,the brightness value(L~*),redness value(a~*)and yellowness value(b~*)are the best from mid-September to mid-October,and the seeds are full and oily;analyzed from the perspective of bioaccumulation,The kernel rate(4.4%)and 100-seed weight(52.4 g)reached the highest value from mid-September to the end of September;from the perspective of chemical composition,alkaloids,flavonoids,saponins and 7 The content of fatty acids is the highest in the species;the Jujube(Ziziphus Jujuba Mill.)in the suitable harvest period and the rush harvest period will not breed aflatoxin under the condition of short soaking(24 h).Correlation analysis results show that spinosin,6’’’-feruloyl spinosin and jujube saponin A are directly related to and promote the increase in brightness and redness of ZSS.Based on the above indicators,it is judged that mid-September to mid-October should be the best harvest time for wild Jujube(Ziziphus Jujuba Mill.).Conclusion:In this study,aiming at the problem of“grabbing green”phenomenon in Ziziphi Spinosae Semen and the content of spinosin is not up to the standard,a comprehensive evaluation study on the quality of ZSS in suitable harvesting period and scrambling harvest period was carried out systematically.The results showed that the best harvest time of Jujube(Ziziphus Jujuba Mill.)was from mid-September to mid-October,and the factors of different producing areas and the inconsistent factors of the collected plants had a greater impact on the quality evaluation.Through the above research,it provides a scientific basis for the authentic quality evaluation of Jujube(Ziziphus Jujuba Mill.)produced in Shanxi,and provides an experimental basis for the technical specifications and local standard compilation of Jujube(Ziziphus Jujuba Mill.).It is very important for the sustainable development of the Jujube(Ziziphus Jujuba Mill.)industry in Shanxi Province.Theoretical value and practical significance. |