Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents / 中国实验方剂学杂志

Objective:To establish a high performance liquid chromatography （HPLC） fingerprint of branches of <italic>Juglans mandshurica</italic> and to evaluate the quality of the samples from different producing areas and in different harvest periods. Method:Chromatographic separation was performed on an Agilent Poroshell 120 SB-C₁₈ column （2.1 mm×100 mm， 2.7 μm） for gradient elution with mobile phase of 0.2% formic acid solution （A）-0.2% formic acid acetonitrile solution （B） （0-5 min， 5%-10%B； 5-25 min， 10%-16%B； 25-40 min， 16%-22%B； 40-45 min， 22%-45%B； 45-50 min， 45%-65%B； 50-52 min， 65%-100%B； 52-55 min， 100%B） at a flow rate of 0.3 mL·min^-1. The column temperature was 30 ℃ and the detection wavelength was 270 nm. The quality of branches of <italic>Juylans mandshurica</italic> was evaluated by similarity evaluation， cluster analysis， principal component analysis and partial least squares-discriminant analysis. The chemical constituents of the samples were identified by HPLC coupled with quadrupole time-of-flight mass spectrometry （HPLC-Q-TOF-MS/MS）. The mass spectrometry was conducted in negative ion mode with electrospray ionization（ESI）. Data were acquired over a range of <italic>m</italic>/<italic>z</italic> 100-1 700 for MS and <italic>m</italic>/<italic>z</italic> 50-1 700 for MS/MS. Result:A total of 19 common peaks were confirmed in 40 batches of samples， and the similarity ranged from 0.430 to 0.995， of which the similarity of samples collected in spring and winter seasons （April， May and December） was greater than 0.90， while the similarity of most samples collected in summer （July to September） was low. Multivariate statistical analysis showed that the samples were divided into two groups according to the harvest time， but there was no obvious classification rule for the samples from different producing areas. The contents of most constituents in the samples collected in spring and winter were higher than those collected in summer. The result illustrated that different harvest periods had great influence on the quality of branches of <italic>J</italic>.<italic> mandshurica</italic>. Compared with the samples collected in summer， the quality of samples collected in spring and winter was better. A total of 22 peaks were proved to be the main constituents that contributed to the difference between samples collected in different seasons. A total of 83 chemical components were identified by HPLC-Q-TOF-MS/MS， including 49 tannins， 7 organic acids， 14 naphthalene derivatives， 1 flavonoid， 6 anthracene derivatives， 2 lignans， 3 diarylheptanoids and 1 saccharide. Totally 13 common peaks were identified. Of the peaks that contributed to discriminate samples collected in different season， 19 peaks were identified and most of them were tannins. Conclusion:The established HPLC fingerprint can provide useful information for the quality evaluation of branches of <italic>J</italic>.<italic> mandshurica</italic>. Tannin is the main constituents in the samples. Harvest period has great influence on the quality of branches of <italic>J</italic>.<italic> mandshurica</italic>.

Study on difference of chemical constituents of Qiai in different harvest periods / 中国中药杂志

Artemisiae Argyi Folium,the dried leaves of Artemisia argyi,has been widely used in traditional Chinese and folk medicines for a long time. Qiai is one of the top-geoherb of Artemisiae Argyi Folium. Trying to investigate dynamic changes of chemical components of Qiai in different harvest periods and explore the optimum harvest time of Qiai,in this study,the contents of total flavonoids and total phenolic acids of 36 batches of Qiai collected in 6 different harvest periods were analyzed by ultraviolet-visible spectrophotometry. Furthermore,an HPLC method was applied for simultaneous determination of eight bioactive compounds including six phenolic acids( 5-caffeoylquinic acid,3-caffeoylquinic acid,4-caffeoylquinic acid,3,4-di-O-caffeoylquinic acid,3,5-di-O-caffeoylquinic acid and 4,5-di-O-caffeoylquinic acid) and two flavonoids( jaceosidin and eupatilin) in Qiai samples. The quantitative results indicated that there were some differences in the contents of total flavonoids,total phenolic acids and bioactive compounds of Qiai samples in different harvest periods. The dynamic changes of total flavonoids and total phenolic acids of Qiai in different harvest periods were consistent. The contents of total flavonoids and total phenolic acids of Qiai samples were higher in the third harvest period( around the Dragon Boat Festival),which is basically consistent with the traditional harvest periods. This present study can provide the basis for determining the suitable harvest time of Qiai,and might be useful for the quality evaluation of this herbal medicine.

Dynamic Variation of the Content of Lignan Glycoside I in Cortex Abizziaeat at Different Harvest Period / 中国药师

Objective:To provide scentific evidence for determining the harvest period of Cortex Abizziae by studying the dynamic variation of the content of lignan glycoside I in Cortex Abizziae.Methods:Chromatography was performed on a Boston Green ODS C18 (250 mm×4.6 mm,5 μm) column,the mobile phase was acetonitrile-0.04% phosphate (18∶82),the flow rate was 1.0 ml·min-1,the detection wavelength was 204 nm,and the column temperature was at 25℃.Results:There were differences in the contents of lignan glycoside I in Cortex Abizziae at different harvest periods.The content of lignan glycoside I reached the highest level in January,decreased quickly from January to March,and gradually increased from April to December.Conclusion:The content of lignan glycoside I in Cortex Abizziae at different harvest periods is different,and the optimum harvest time of Cortex Abizziae is determined from November to January of the following year.

Optimum harvest time of Tulipa edulis based on comparison of biomass accumulation and medicinal quality evaluation / 中国中药杂志

The optimum harvest time of Tulipa edulis was explored based on biomass accumulation and medicinal quality evaluation. Samples were taken from bud stage (Feb 13th) to dormancy stage (May 14th) and the growth indexes, organs biomasses, drying rate, contents of water-soluble extract and polysaccharides were determined. The results showed that biomass distribution of T. edulis varied with growth center and the bulb gained maximum biomass allocation in the whole growth period. The total biomass accumulation and bulb biomass accumulation　increased in the whole growth period and peaked in fructescence stage. No differences were observed in bulb biomass among fructescence stage, withering stage and dormancy stage. The correlation between bulb biomass allocation and other morphological indexes varied with the harvest time. Bulb dry weight biomass had negative correlation with some morphological indexes of aerial part of T. edulis at bud stage, flower stage and fructescence and had significant positive (P<0.05) or extremely significant positive correlation（P<0.01）with other morphological indexes except for root at bearing fruits stage. The drying rate of bulb of T. edulis increased with the extension of harvest time and peaked in dormancy stage. The water-soluble extract of T. edulis bulb was the highest in pre-growing-stage. The tendency of polysaccharides contents showed a W-shape variation during the harvesting period. The polysaccharides content was the lowest in fructescence stage and was the highest in dormancy stage. Considering the yield and medicinal quality of T. edulis bulb, the optimum harvest time of T. edulis is in the withering stage or early stage of dormancy.

Determination of Chlorogenic Acid in Honeysuckle Stem and Honeysuckle from Different Sources in Differ-ent Harvest Periods by HPLC / 中国药师

Objective:To establish an HPLC method for the determination of chlorogenic acid in honeysuckle stem and honeysuck-le from different sources in different harvest periods. Methods:A Waters C18 column(250 mm × 4. 6 mm,5 μm)was used. The mo-bile phase consisted of acetonitrile-0. 4% H3 PO4(10:90)with the flow rate of 1. 0 ml·min-1 . The detection wavelength was 327 nm and the column temperature was 30℃. An external standard method was established for the determination of chlorogenic acid in honey-suckle stem and honeysuckle in six different harvest periods from three sources. Results:There was a good linear relationship within the range of 0. 065-1. 300 μg for chlorogenic acid(r=0. 999 8). The content of chlorogenic acid in honeysuckle was the highest in Sep-tember and October. The content of chlorogenic acid in Lonicera acuminata was the highest among the honeysuckle stem from three dif-ferent sources. Conclusion:The content of chlorogenic acid in honeysuckle has a certain relationship with the harvest time,which can provide theoretical basis for the choice of harvest time for honeysuckle stem.