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Determination Of Active Components And Metal Elements In Shengmaiyin And The Analysis Of Pesticide Residue

Posted on:2011-07-06Degree:MasterType:Thesis
Country:ChinaCandidate:C LiangFull Text:PDF
GTID:2144360305458324Subject:Drug analysis
Abstract/Summary:PDF Full Text Request
ObjectiveTo determine the active components and the metal elements and analysis the pesticide residue in Shengmaiyin, it can provide the basis of quality control for Shengmai san.Methods1,The optimal alcohol extraction process of Shengmaiyin was studied by orthogonal design with extractive yield and the contents of y-schizandrin.Four factors were investigated in this experiment, including the concentration alcohol, the solvent consumption, time of extraction and times of extraction. RP-HPLC method was established to determineγ-schizandrin in Shengmaiyin.And determined y-schizandrin and three ginsenosides in different form of Chinese patent medicines of Shengmaiyin. y-schizandrin and three ginsenosides of Shengmai san were indentified by TLC.2,Atomic absorption spectrometry (AAS) was established to determine Ca,Mg,Zn,Cu,Fe,Mn,K,Na,Cd nine metal elements in Shengmaiyin in order to compare the content of ginseng shengmaiyin and Tangshen shengmaiyin.3,GC was established to determine Dichlorvos,α-BHC,β-BHC, pp'-DDE, pp'-DDD, Quintozene, Chlorpyrifos, parathion-methyl, parathion, fenpropathrin and permethrin 11 pesticides residue. It can restrict the content of objectionable constituent which is harmful to human body. Results1,The results showed that the optimal extracting condition was 85% alcohol consummated 10 times the amount of material, refluxing for once and 1.5 hour each time. RP-HPLC method was established to determineγ-schizandrin in Shengmaiyin. The separation was achieved on a Diamonsil C18 column (250 mm×4.6 mm,5μm), using solvents of methanol-acetonitrile-H2O (50:30:20,v/v/v) as mobile phase. It was detected at 254 nm with flow rate as 1.0 mL·min-1, the column temperature was room temperature and sample size was 20μL. The results indicated that the calibration curve was linear in the range of 1-80μg·mL-1 forγ-schizandrin(r=0.9994), average recovery was 97.8% and RSD was 1.7%. TLC method was established to indentifyγ-schizandrin and three ginsenosides of Shengmai san.The results indicated that the method is simple and fast for qualitation analysis.2,Compared the effects of three extraction methods.which were dip-molding, decocting and Ultrasonic method,to extraction yield. We choosed decocting method to extract shengmai san.Compared the two digestion systems of constant temperature program and linear temperature program,the results indicated that linear temperature program is better. The result indicated that linear correlation, precision and recovery of eleven elements were all correspond to detection request.3,The determination of pesticides residue in eight samples using liquid-liquid extraction was established.Among all the samples,three of them were detected organchlorine pesticide,but the results all below the limit of detection. The results indicated that the calibration curve of eleven pesticides were linear, correlation coefficient were all higher than 0.9962,recovery range of samples within 80-120%.The results showd that the method is suitable for the determination of shengmaiyin and it's patent medicine.ConclusionThe assay methods were accurate and with good reproducibility and can provide a quantitative basis for the quality assessment for shengmaiyin.
Keywords/Search Tags:Shengmaiyin, extraction technology, metal elements, pesticide residue
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