Fructus Corni Processing Process Monitoring And Quality Control Research

Fructus Corni is the dry ripe fruit of Cornaceae plant Cornus officinalis sieb.et Zucc. It is a precious Chinese herbal medicine, and has been a hot spot in the field of modern medical treatment and healthy food. Fructus Corni is often processed with wine in clinics, which could tonify liver and kidney. Research shows that after processing efficacy components (such as amino acids, iridoid) of Fructus Corni are reduced, such as organic acid and 5-HMF increased. In this thesis both traditional and modern chemical analysis methods were used, to study the changes of the chemical compositions during the processing of Fructus Corni to clarify the mechanism of processing, and provide a basis for improving quality of crude and processed Fructus Corni.1. Quality control of processed Fructus Corni with traditional methodTraditional method for assessing quality of processed Fructus Corni, including identification traits, determination of moisture, ash and extract content, TLC chromatography for identification of ursolic acid and loganin in wine processed Fructus Corni, HPLC chromatography to determine content of loganin and gallic acid. Choose three batches of wine steamed Fructus Corni as samples to assess the quality, results showed that the characteristics were qualified, all the three batches of herbs containing ursolic acid and loganin, content of moisture, ash and extract were qualified, content of loganinwas also qualified,which showed that all the three batches of samples were qualified. In order to verify the quality of processed Fructus Corni further. We also determined contents of gallic acid, polysaccharides, total flavonoids, total organic acids, total saponins in each batch of Fructus Corni. The results showed that three batches of Fructus Corni were good, uniform and of stable quality.2. Analysis of Fructus Corni by Infrared Spectroscopy during processingInfrared Spectrum technology was adopted to carry out the analysis of macro and fingerprint characteristics of infrared spectrum of Fructus Corni. Fructus Corni was processed by steaming with wine for 48 h. During processing, samples processed at different time points were collected to carry out infrared spectrum analysis. It could be deduced from the spectra that there were alcohols, organic acids, esters and so on in Fructus Corni. When being processed, the amounts of components changed slightly and stabilized gradually with main peaks at 3309 cm-1, 1713 cm-1 and 1028 cm-1. During processing, the content of amine-group compounds showed an downward trend in 0-24 h, and in 24-48 h the spead of decreasing become slow, therefore 18～24 h could be regarded as the optimal processing time. This Infrared Spectroscopy method is simple and convenient to analyze Fructus Corni samples during processing, and can preliminary recognize the main ingredients in samples. It could provide useful references for the optimization of processing of Fructus Corni.3. Analysis of Fructus Corni by GC-MS during processingThis part was to study the chemical constituent changes of Fructus corni before and after processing by GC-MS. Fructus corni was processed with wine steaming for 0-48 h, and then extracted and methyl esterified for sample preparation. Samples of wine processed Fructus Corni during 0-48 h were analyzed by GC-MS of the chemical compositions. Volatile constituent of Fructus corni of different processing times were analyzed by GC-MS. More than 60 components were isolated, among which 35 components were identified. Relative content of each peak were calculated, The main components are methyl paraben, citric acid trimethyl ester, nonanedioic acid dimethyl ester,1,2,3-Propane tricarboxylic acidl-hydroxy-trimethyl ester, methyl tetradecanoate,2-Propenoic acid 3-(4-hydroxyphenyl)-methylester,4-methyl-1,6-heptadiene-4-ol, 9-hexadecenoic acid methyl ester, hexadecenoic acid methyl ester, dibutyl phthalate esters, and so ori. This infrared spectroscopy method is simple and convenient to analyze Fructus corni samples during processing and can preliminary recognize the main ingredients during processing. It could provide useful references for the optimization of processing of Fructus corni.4. Dynamic analysis of HPLC and UFLC-TOF-MS during processing of Fructus CorniThis part was to establish HPLC and UFLC-TOF-MS methods to compare the dynamic process of chemical compositions during processing of Fructus Corni. The HPLC analysis was carried out on a Kromasil C18 column (4.6 mm×250 mm,5μm), with the mobile phase consisting of acetonitrile-water (7:93) in isocratic elution for 5-(hydroxymethyl) furfural and acetonitrile-water (15:85) in isocratic elution for loganin; The UFLC-TOF-MS analysis used negative ion detection mode in Shimadzu UFLC liquid system by AB SCIEX Triple TOFTM5600 mass spectrometer with the mobile phase consisting of acetonitrile-0.01% aqueous acetic acid in gradient elution. We found that the contents of 5-HMF, loganin, quercetin and etc. in Fructus Corni changed significantly under different processing time by using HPLC and mass spectrometry. HPLC has significant advantage in detecting some compounds in Fructus Corni, while other chemical compositions in Fructus Corni has good response to HPLC coupled with mass spectrometry in negative ion detection mode. This provides a new approach for analyzing changes of chemical components during processing of Fructus Corni and also for quality control of the products. And these two methods can be used together to comprehensively understand the mechanism of processing of Fructus Corni, and finally give advice to the production of Fructus Corni.