| Objectives: Through the research on the extraction,concentration,drying and molding,the preparation technology of Lycium barbarum L.granules was completed.Then,we determine its preparation process,pilot scale,study on its quality standards,and draft quality standards.That is conducive to Lycium barbarum L.formula granules particles for the review of the record to provide research methods and theoretical basis.Methods: According to the “Quality control and standard formulation requirements of TCM formula granules(draft for soliciting opinions)” and the preparation specifications,the following tests were mainly carried out.First,it is the quality of raw Chinese wolfberry slices,including according to the pharmacopoeia items of the total examination and water-soluble solid yield determination.Secondly,the research of preparation technology is divided into six parts.(1)The content of betaine and the yield of solid were used as the indexes in the extraction process.The factors of soaking time,amount of water,decocting time and times of decocting were screened by single factor,and then the best extraction process was selected by orthogonal test design.(2)According to the retention rate of betaine content,the concentration methods at normal pressure and reduced pressure were optimized.(3)The method of drying(atmospheric pressure and vacuum)and the thickness of paving plate(0.4,0.8,1.2 cm)were investigated.(4)Taking the forming rate,moisture absorption rate and solubility as the index,the comprehensive weighted coefficient scoring method was used to investigate the type and ratio of auxiliary materials for wet and dry granulation.And the primary forming rate was taken as the index in dry granulation.Single factor investigation and orthogonal test were carried out to optimize the process parameters of dry granulator(feed,tablet pressing,granulation frequency).The total mixing process conditions are set at different times,and the minimum mixing time is determined according to the appearance of the color of the auxiliary materials and the main medicine.The loading amount of the particles is calculated according to the prescribed dosage of Chinese wolfberry slices in the Pharmacopoeia and the paste yield in this experiment.The critical relative humidity is obtained by drawing the critical relative humidity curve according to the hygroscopicity of the particles in different saturated salt solutions.(5)According to the results of the above screening,the preparation process is decided to enlarge three batches of pilot-scale samples.(6)Through the correlation study of the characteristic map of quality transfer,the characteristic maps of the same batches of prepared slices,extract,concentrated extract,dry extract and formula granules were determined,and the retention of components in each intermediate was evaluated according to their similarity.(7)The storage conditions and shelf life were determined by stability study,influence factor test,accelerated test and longterm test.Third,the study of quality standards,with three batches of samples as the study object,to establish its quality standards,including name,source,preparation,character,identification,inspection,extract,characteristic atlas,content determination,specification,storage,at the same time attached to the quality standard drafting instructions.Third,it is the study of quality standards.The quality standards of three batches of samples were established,including name,source,preparation,character,identification,examination,extract,characteristic atlas,content determination,specification and storage,at the same time attached to the quality standard drafting instructions.Results: First,the quality test results of 15 batches of crude drugs from Ningxia,Qinghai and Gansu were all in accordance with the Pharmacopoeia,and the water-soluble solid content should not be less than 49.7% as the selected standard.Second,the best preparation technology is to take the slices of Chinese wolfberry and decoct them three times,adding 8 times water in the first time,soaking time 1.5h,decocting time 1h,and filtrating the decoction through 200 mesh sieve;In the second and third time,adding 6 times water,decocting for 1 H,the decoction was filtered by 200 mesh sieves respectively and combined with the filtrate three times.The filtrate is then concentrated under reduced pressure(temperature: 60℃,vacuum:-0.07 ～ 0.085MPa)to a consistency of 1.20～1.25(60℃).It is then dried in vacuum(temperature: 60 ℃,vacuum degree:-0.06 ～ 0.085 MPa)and the thickness of the paving plate does not exceed 0.8cm.Next,it is dried in vacuum(temperature: 60 ℃,vacuum:-0.06 ～ 0.085 MPA),the thickness of the paving plate is not more than 0.8 cm,then the dry extract is taken and crushed through80 mesh sieve.Dry extract powder was mixed with 30% β-cyclodextrin(through 80 mesh sieve)and 0.1% magnesium distearate for 5 min.KCG-25 B intelligent granulator was used,the pressure was set to 3-3.5 mpa(normal granulating parameters),the first stage granulating was2.0 mm,the second stage granulating was 1.8 mm screen,the feeding frequency was 10 Hz,the pressing frequency was 20 Hz,and the granulating frequency was 20 Hz.The particles obtained by dry pressure test between No.1 and No.5 sieves are qualified particles and are packed below82% Critical relative humidity in 5g bags.The correlation results of the characteristic map of quantity and quality transfer showed that the prepared formula granules retained the components contained in the prepared slices.Stability research data are still being collected.Thirdly,the quality standard of Lycium barbarum L.formula granules was established.It was identified by TLC,HPLC characteristic chromatogram was established,7 characteristic peaks were defined,and HPLC method for determination of betaine was established.At the same time,the contents of the above quality standards are drafted and explained in detail.Conclusion: The formula granules of Lycium barbarum L.were prepared in this paper,and the preparation technology was confirmed by pilot scale up.The parameters were clear,stable and feasible,and the quality was controlled,the results provide reference for the production and quality control of Lycium barbarum L.formula granules. |
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