ABSTRACT
To study the effects of different drying methods on the quality of male flowers of Eucommia ulmoides(MFOEU), we treated fresh MFOEU samples with drying in the shade(DS), vacuum freeze drying(VFD), high-or low-temperature hot air drying(HTHAD, LTHAD), microwave drying(MD), and vacuum drying(VD), respectively. The color, total flavonoid content, total polysaccharide content, and main active components such as geniposide, geniposidic acid, rutin, chlorogenic acid, galuteolin, pinoresinol diglucoside, and aucubin in MFOEU were taken as the evaluation indicators. The quality of MFOEU was comprehensively evaluated by entropy weight method combined with color index method, partial least squares discriminant analysis and content clustering heat map. The experimental results showed that VFD and DS basically kept the original color of MFOEU. The MFOEU treated with MD had higher content of total polysaccharides, phenylpropanoids, lignans, and iridoids. The MFOEU treated with LTHAD had higher content of total flavonoids and that treated with VD had lower content of active components. According to the results of comprehensive evaluation, the quality of MFOEU dried with different methods followed the order of MD>HTHAD>VFD>LTHAD>DS>VD. Considering the color of MFOEU, the suitable drying methods were DS and VFD. Considering the color, active components, and economic benefits of MFOEU, MD was the suitable drying method. The results of this study are of a reference value for the determination of suitable methods for MFOEU processing in the producing areas.
Subject(s)
Eucommiaceae/chemistry , Flowers/chemistry , Flavonoids/analysis , Rutin/analysis , Chlorogenic Acid/analysisABSTRACT
This study aims to develop the pre-column derivatization high performance liquid chromatography(HPLC) method for the determination of 16 kinds of amino acids in Eucommia ulmoides leaves, and compare the content of amino acids in the leaves harvested at different time and under leaf-oriented cultivation mode(LCM) and arbor forest mode(AFM). The HPLC conditions are as below: phenyl isothiocyanate(PITC) as pre-column derivatization agent, Agilent ZORBAX C_(18 )column(4.6 mm×250 mm, 5 μm), mobile phase A of acetonitrile-water(80∶20), mobile phase B of 0.1 mol·L~(-1) sodium acetate solution-acetonitrile(94∶6), gradient elution, flow rate of 1.0 mL·min~(-1), injection volume of 5 μL, column temperature of 40 ℃, and detection wavelength of 254 nm. The HPLC profile indicated well separation of 16 kinds of amino acids and the amino acid content in E. ulmoides leaves was up to 16.26%. In addition, the amino acid content in leaves of E. ulmoides under LCM was higher than under AFM. The amino acid content varied with the harvesting time. Through orthogonal partial least squares discriminant analysis, the amino acids of E. ulmoides under LCM and AFM were compared, which can distinguish the leaves under LCM from those under AFM. Principal component analysis was applied to comprehensively score the amino acids of E. ulmoides leaves. The results showed that the score of leaves under LCM was higher than that under AFM. Nutritional evaluation results indicated that the proteins in E. ulmoides leaves belonged to high-quality vegetable proteins. The established method for the determination of amino acid content is reliable. With the amino acid content as index, the leaf quality of E. ulmoides under LCM is better than that under AFM. This study lays a theoretical basis for the promotion of LCM for E. ulmoides and the development of medicinal and edible products from E. ulmoides leaves.
Subject(s)
Amino Acids/metabolism , Eucommiaceae/chemistry , Chromatography, High Pressure Liquid/methods , Plant Leaves/chemistryABSTRACT
Objective:The volatile components of Rhododendri Mollis Flos were determined and the differences of volatile components at different flowering stages were compared and analyzed. Method:Gas chromatography-ion mobility spectrometry （GC-IMS） was used to detect the volatile components in Rhododendri Mollis Flos at different flowering stages （bud stage， initial flowering stage， half-flowering stage， blooming stage and late blooming stage）. GC-IMS spectra combined with cluster analysis， principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） were used to compare the differences and similarities of volatile components in different flowering stages. Result:A total of 70 volatile components in Rhododendri Mollis Flos at different flowering stages were detected， among which 67 were common components， and 47 were identified qualitatively， mainly alcohols， esters and aldehydes. Carveol was a special component at the late blooming stage. The content of alpha-terpineol is the highest at the initial flowering stage， but not at the blooming stage and late blooming stage. The relative contents of the active ingredients ［6-methyl-5-hepten-2-one， nonanal， alpha-terpineol， 1，8-cineole， linalool oxide， 1-octen-3-ol， （<italic>E</italic>）-3-hexenol］ showed a decreasing trend during flowering stages. GC-IMS spectra showed that the samples at different flowering stages had their own characteristic peak regions， and also had common regions. The results of cluster analysis， PCA and OPLS-DA all showed that the samples at different flowering stages were distinguishable. OPLS-DA was used to screen 19 different components to distinguish different flowering stages， including <italic>γ</italic>-butyrolactone， 1，8-cineole， ethyl hexanoate， etc. Conclusion:Rhododendri Mollis Flos samples at different flowering stages can be distinguished obviously， and the active substances in the volatile components are gradually dissipated with the degree of flower opening， which can provide reference for the improvement of material basis and the study of different flowering stages of Rhododendri Mollis Flos.
ABSTRACT
Objective:To analyze and identify the flavonoids of Citri Reticulatae Pericarpium with different aging time by an ultra-performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry （UPLC-Q-Orbitrap HRMS）. Method:Compounds were separated on Agilent Extend-C<sub>18</sub> column （3.0 mm×100 mm， 1.8 μm）， mobile phase was 0.1% acetic acid aqueous solution （A）-0.1% acetic acid methanol solution （B） for gradient elution （0-25 min， 5%-95%B； 25-30 min， 95%B； 30-30.1 min， 95%-5%B； 30.1-35 min， 5%B）， the flow rate was 0.4 mL·min<sup>-1</sup>， and the column temperature was set at 30 ℃. High resolution mass spectrometry was performed with electrospray ionization （ESI）， and scanned in positive and negative ion modes by means of full scan/data dependent secondary scan （Full MS/dd-MS<sup>2</sup>）. The multistage ion fragment information combined with mzCloud network database， local high resolution mass spectrometry database of traditional Chinese medicine components （OTCML）， literature information and relevant reference materials were used for accurate qualitative analysis. Result:Totally 43 flavonoids in Citri Reticulatae Pericarpium were identified， including 24 flavones， 5 flavonols， 13 dihydroflavones and 1 chalcone. The flavonoids in samples with different aging time were basically consistent in material types， but the peak area was different. According to the comparison of relative content in the peak area， it was found that the relative contents of 30 flavonoids showed an overall increasing trend with the increase of aging time. Among them， the relative contents of 24 flavonoids （such as hesperidin， diosmin， 6-demethoxytangeretin， nobiletin and tangeretin） increased significantly. There was no significant change in the relative contents of the other 13 flavonoids （such as naringenin and neohesperidin）. Conclusion:An efficient method is established in this paper to identify flavonoids in Citri Reticulatae Pericarpium with different aging time and their relative content changes rapidly and accurately. The findings provide a methodological reference for the study on pharmacodynamic material base and quality control of Citri Reticulatae Pericarpium， and it provides experimental basis that drugs processed long time ago have better effect of Citri Reticulatae Pericarpium.
ABSTRACT
In this paper， through the collection and collation of ancient materia medica， medical books and medical formulary， combining with modern literature， the historical changes of the name， origin， position， harvesting time， medicinal parts， toxicity， functions and indications， processing methods of Rhododendri Mollis Flos （RMF） were systematically combed and verified， so as to provide reference for clinical application， processing standard and basic research of RMF. According to textual research， RMF is the dried flower of Rhododendron molle. In each historical period， there are many aliases and local names， being with phenomenon of homonyms and synonyms. RMF is mostly wild and planted in a small amount， harvesting time is mostly in March to April. However， the harvesting flowering period is differently described as initial bloom， full bloom and extensive bloom. RMF was first recorded in Shennong Bencaojing (《神农本草经》)， but it did not mention its medicinal parts. Then the flowers， fruits， roots are be used as medicine， but flowers are still the main medicinal parts. RMF had a long processing history， included fried， vinegar-fried， wine-fried， steamed， wine-steamed， vinegar-steamed， and many other processing methods in ancient times. However， at present， only raw products are used in clinical practice， and only a few modern books retain the methods of stir-fried and wine-steamed， believing that the processing can reduce toxicity of RMF.
ABSTRACT
Objective To establish a UPLC fingerprint of Cassiae Semen from two species which is expected to provide standard for the quality control and evaluation. Methods Chromatography conditions were Agilent ZORBAX EP C18 (100 mm × 3.0 mm, 1.8 μm) column with gradient mobile phase of acetonitrile-0.01% formic acid solution. UV detection wavelength was 285 nm, the flow rate was 0.4 mL/min, the column temperature was 30 ℃ and the sample quantity was 1 μL. Results The common mode of UPLC fingerprint of Cassiae Semen was established firstly. There were 20 common peaks had been calibrated by similarity evaluation. Seven peaks had been identified by comparing retention time with UV spectrum analysis. The similarity evaluation of 20 batches samples of Cassiae Semen was more than 0.9. Twenty batches of Cassiae Semen could be divided into four grades when the sum of squared Euclidean distance is 5 become the result of Cluster Analysis. Principal component analysis got three principal components through dimension reduction. The results of principal component scores agree with the clustering analysis. By fitting the load factor model of the first principal component, characteristic peak such as rubrofusarin-6-O-β-gentiobioside were filtered to appraise Cassiae Semen's quality. Conclusion The contents of same chemical compositions between Cassia obtusifolia and C. tora are different. UPLC fingerprint can be used in Cassiae Semen's quality control and evaluation.
ABSTRACT
To investigate the dynamic change rules of volatile components from Atractylodis Macrocephalae Rhizoma with different stir-baking degrees (from slight stir-baking, stir-baking to yellow, stir-baking to brown, to stir-baking to scorch). In the present experiment, the Atractylodis Macrocephalae Rhizoma samples with different stir-baking degrees were collected at different processing time points. The contents of volatile oil in various samples were determined by steam distillation method, and the volatile compounds were extracted by using static headspace sampling method. Gas chromatography-mass spectrography (GC-MS) and automated mass spectral deconrolution and identification system (AMDIS) were combined with Kováts retention index to analyze the chemical constituents of the volatile compounds. The results showed that with the deepening of the stir-baking degree, the content of volatile oil was decreased step by step in 4 phases, and both the compositions and contents of volatile components from Atractylodis Macrocephalae Rhizoma showed significant changes. The results showed that the dynamic change rules of volatile components from Atractylodis Macrocephalae Rhizoma in the process of stir-baking were closely related to the processing degree; in addition, Atractylodis Macrocephalae Rhizoma and honey bran had adsorption on each other. These results can provide a scientific basis for elucidating the stir-baking (with bran) mechanism of Atractylodis Macrocephalae Rhizoma.
ABSTRACT
This study is to explore the reason of "the older, the better" of PCR and itsincrease of flavonoids. We identified the fun- gus isolated from the PCR using microscopic and molecular identification. HPLC method was used to determine the content of 4 fla- vonoids and to clarifythe regularity of them; UV spectrophotometry method was used to determine the total content of flavonoids; reverse thinking was applied to screen the fungus that have close relation to the change of flavonoids. Finally, we have isolated and identified 25 fungusfrom the PCR, which belong to 2 genus and 4 species, including pencillium commune, P. minioluteeum, P. citrinum, Aspergillus flavus and A. niger. The content of flavonoids was increased in the mildew PCR due to A. niger and other fungus. Therefore, "the ol- der, the better" of PCR had its scientific reason that the increase of flavonoids had a close relation of the metabolic activity of A. niger and other fungus.
Subject(s)
Citrus , Chemistry , Microbiology , Flavonoids , FungiABSTRACT
<p><b>OBJECTIVE</b>To establish a derivative fluorometry method for the determination of sulfur dioxide residues in traditional Chinese medicine.</p><p><b>METHOD</b>The optimal derivation condition was established. The fluorescence intensity was detected at excitation wavelength of 321 nm, and emission wavelength of 384 nm.</p><p><b>RESULT</b>A linear relationship was obtained between the fluorescence intensity and the addition of reference substance in the range of 0.999 7-17.99 nmol with a correlation coeffient of 0.999 9, and the average recovery was 102.3% with RSD 4.6%.</p><p><b>CONCLUSION</b>This method is simple and sensitive with quick and correct result. It can provide a reference for the determination of sulfur dioxide residues in traditional Chinese medicine.</p>
Subject(s)
Drugs, Chinese Herbal , Fluorescence , Medicine, Chinese Traditional , Sensitivity and Specificity , Species Specificity , Spectrometry, Fluorescence , Methods , Sulfur Dioxide , TemperatureABSTRACT
This experiment shows how to use the automated mass spectral deconvolution & identification system (AMDIS) to deconvolve the overlapped peaks in the total ion chromatogram (TIC) of volatile oil from Chineses materia medica (CMM). The essential oil was obtained by steam distillation. Its TIC was gotten by GC-MS, and the superimposed peaks in TIC were deconvolved by AMDIS. First, AMDIS can detect the number of components in TIC through the run function. Then, by analyzing the extracted spectrum of corresponding scan point of detected component and the original spectrum of this scan point, and their counterparts' spectra in the referred MS Library, researchers can ascertain the component's structure accurately or deny some compounds, which don't exist in nature. Furthermore, through examining the changeability of characteristic fragment ion peaks of identified compounds, the previous outcome can be affirmed again. The result demonstrated that AMDIS could efficiently deconvolve the overlapped peaks in TIC by taking out the spectrum of matching scan point of discerned component, which led to exact identification of the component's structure.