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OBJECTIVE To establish a comprehensive and rapid m ethod for the a nalysis of chemical constituents as phthalides and organic acids in Angelica sinensis ，and to provide scientific reference for the quality evaluation and pharmacodynamic substance research of A. sinensis . METHODS The 70％ ethanol extract of A. sinensis was analyzed by ultra high performance liquid chromatography-quadrupole-time of flight tandem mass spectrometry （UPLC-Q-TOF/MS）. The determination was performed on ACQUITY UPLC BEH-C 18 column with mobile phase consisted of 0.1％ formic acid solution- acetonitrile（gradient elution ）at the flow rate of 0.3 mL/min. The column temperature was set at 30 ℃，and sample size was 2 µL. The ion source was an electrospray ion source ，using positive ion scanning mode ，and the mass scanning range was m/z 50-1 000. Capillary voltage was 4 000 V； atomizer pressure was 35 psi；cracking voltage was 135 V and the taper hole voltage was 65 V；the temperature of dry gas was 320 ℃；the flow of dry gas was 10 L/min and the flow of sheath gas was 11 L/min；collision energy were 20 and 40 V. Qualitative Analysis 10.0 software was used to obtain the retention time of compounds ，the accurate mass number of excimer ion peaks and secondary fragments. The compounds were analyzed by comparing with the mass spectra of the reference substance ，combined with relevant literature ，mass spectrometry cleavage law and database such as Chemspider ，MassBank，PubChem. RESULTS A total of 72 compounds were identified or deduced from A. sinensis ，including 55 phthalides，13 organic acids and 4 other constituents. CONCLUSIONS The established method is rapid and accurate for the identification of chemical constituents from A. sinensis ，such as organic acids and phthalides ，which provides an efficient and rapid analytical method for the comprehensive characterization of its chemical constituents.
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Objective: To study the phthalides with vasodilating activity of alcohol extracts from stems and leaves of Ligusticum chuanxiong. Methods: Compounds were isolated by extensive chromatographic techniques including MCI, silica gel, Sephadex LH-20, ODS, and semi-preparative HPLC. The vasodilating effect of phthalide and dimer phthalide on thoracic aortic ring in vitro was investigated. Results: Ten phthalides were isolated and identified, and their structures were elucidated as Z-3-butylidenephthalide (1), senkyunolide-E (2), Z-senkyunolide-H (3), (3Z,7β)-3-butenyl-7-hydroxy-4,5,6,7-tetrahydrophthalide (4), neoligustilide (5); Z,Z’-3.3’a,7.7’a-diligustilide (6), 3Z,3Z’-6,8’,7,3’-diligustilide (7), Z-tokinolide A (8), (3’Z)-(3S,8R,3a’S,6’R)-4,5-dehydro-3.3’a,8.6’-diligustilide (9), and (3Z)-(3aR,6S,3’R,8’S)-3a.8’,6.3’-diligustilide (10). Compound 1, 6-9 significantly reduced the strain of thoracic aortic ring in KCl preconstricted rats. The diastolic rate of compounds 6-8 were 60%, 52% and 70% at the highest concentrations (12 μmol/L), respectively. The EC50 was 9.46, 11.86 and 8.73 μmol/L, respectively. Firstly isolated from the stems and leaves of L. chuanxiong. Compounds 6, 8 are firstly isolated from L. chuanxiong. The test compounds could dilate blood vessels, and the activity of dimer phthalide was better than that of phthalide.
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Objective: In order to establish a rapid and efficient analysis method for identification of the complex components in Jingzhi Guanxin Soft Capsule, and provide the basic research data for the systematic elaboration of its chemical constituents. Methods: An ultra-high performance liquid chromatography-quadrupole/Orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was used for the identification analysis of the components in Jingzhi Guanxin Soft Capsule, and the multistage fragments ions data was compared with the standard substance and literature consulting. Results: Forty-three compounds were identified in this study, including flavones, phthalides, organic acids, quinones and other categories. Conclusion: The chemical constituents of Jingzhi Guanxin Soft Capsule are identified systematically, accurately and efficiently, which provide the theory basis for the further research of its pharmacodynamic material basis and quality control.
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Objective: To clarify the chemical constituents of Tiandan Tongluo Capsule and establish a precise and effective identification method for the complex composition of TCM. Methods: This objective was achieved mainly depending on the information of the accurate mass and the multistage fragment ions obtained by ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS), comparing the relative retention time and the mass spectrometric data of the standard substance and consulting the reference literature. Results: Forty compounds were identified in this study, including the phenoliacids, anthraquinones, flavones, phthalides, fatty acids, and the others. Conclusion: This study can identify various chemical constituents of Tiandan Tongluo Capsule systematically, accurately, and rapidly. Moreover, the scientific theory basis will be provided for the pharmacodyamic material basis and the quality control of this drug at the same time.
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Objective In order to clarify the chemical constituents in traditional Chinese medicine (TCM) compound preparation of Danhuang Quyu Capsule and establish an efficient analysis method for the identification of the complex components in TCM accurately and rapidly. Methods An ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) was used to perform an identification analysis of the chemical constituent in the Danhuang Quyu Capsule.This objective was achieved mainly depending on the information of the accurate mass and the multistage fragment ions obtained by UPLC-Q-Orbitrap, comparing the relative retention time and the massspectrometricdata of the standardsubstance and consulting the reference literature. Results Fifty nine compounds were identified in this study, including the flavones, phthalides, anthraquinones, alkaloids, monoterpene glycosides, organic acids, and other categories. Conclusion This study can identify various chemical constituents of Danhuang Quyu Capsule systematically, accurately and rapidly. What's more, the scientific theory basis will be provided for thepharmacodyamic material basis and the quality control of this drug at the same time. Key words: Danhuang Quyu Capsule; UPLC-Q-Orbitrap HRMS; flavones; phthalides; monoterpene glycosides
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Objective To separate and identify the chemical constituents in Liujing Toutong Tablets (LTT) by HPLC-Q-TOF/MS. Methods The main components were separated by using the gradient elution method with RP-HPLC, Diamonsil C18 (250 mm × 4.6 μm, 5 μm). The positive and negative electro spray ionization (ESI) source was adopted for determine the chromatographic effluent, the main chromatographic peaks are assigned and distinguished by Q-TOF. These components were further analyzed by accurately relative molecular mass of compounds, and Combined with Positive and negative ions MS information and related literature data. Results According to the MS principle, the corresponding reference substances and literature datas, Ninety-five compounds of LTT were identified, mainly including isoflavones, coumarins, iridoids and phthalides. Furthermore, all of the constituents were surveyed and classified according to their medicinal materials derivation. Conclusion In this study, the main components in LTT were elucidated completely by HPLC-Q-TOF/MS. The results could provide the evidence for the research on active constituents and quality control of LTT.
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To provide a scientific basis for the selection and optimization of the modern drying processing method for Angelicae Sinensis Radix (ASR). Three phenolic acids (esters), 6 phthalides were determined by using UPLC-PDA while polysaccharides were determined by UV-Vis spectrophotometry. Then the effects of drying methods on the inner qualities of ASR were evaluated through principle components analysis (PCA) combined with the appearance properties after drying. Results showed that the contents of chlorogenic acid and ferulic acid in samples obtained with controlled temperature and humidity drying (CTHD), medium and shortwave infrared drying (MSID) and microwave vacuum drying (MVD) methods were significantly higher than those with primary drying processing(PDP) method and the fresh samples. Multivariate statistical analysis showed that samples processed with CTHD had more similar general chemical properties with those processed with PDP, suggesting that CTHD was appropriate for the modern primary drying processing of ASR. With samples processed with traditional PDP method as reference, the CTHD method was further optimized in the processing parameters for ASR by orthogonal experiment design. Considering the consumption of drying power and time and other parameters, the modern drying parameters for the primary drying processing of ASR were finally optimized as follows: controlled temperature and humidity drying at 40-45 ℃, relative humidity below 25% and target moisture content about 50% in the first stage of drying process, tempering for 12-24 h, and then drying under the conditions of temperature at 50-60 ℃, relative humidity below 20% and fan frequency at 30-40 Hz in the second stage. The study provided the scientific evidence for the selection of appropriate drying method and suitable parameters for the modern primary drying processing of ASR, as well as the beneficial exploration and practice on the formation of technical standard of primary drying processing for roots and rhizomes types herbal medicines.
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Through literature analysis, this paper summarizes the application of Angelicae Sinensis Radix in depression. The organic acids, phthalides, and polyacetylenes of Angeliae Sinensis Radix have the effect of antidepression, neuroprotective and monoamine reuptake inhibition. This paper reviewed that Angelicae Sinensis Radix improved the possible mechanisms of depression including injury of nerve, oxidative stress, and neurotransmitter system disorders, which will provide scientific basis for clinical treatment of depression.
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The phytochemical progress on Angelica sinensis (Oliv.) Diels over the past decades is summarized. Since 1970s, 165 chemical constituents, including phthalides, phenylpropanoids, terpenoids and essential oils, aromatic compounds, alkaloids, alkynes, sterols, fatty acids, and polysaccharides have been isolated or detected from the various parts of the title plant.
Subject(s)
Alkaloids , Alkynes , Angelica sinensis , Chemistry , Benzofurans , Fatty Acids , Oils, Volatile , Phytochemicals , Phytosterols , Polysaccharides , Propanols , TerpenesABSTRACT
Objective To study the preparation technique of Apium graveolens L.capsules and to assess the quality of the prepared capsules. Methods and Results Using moldability and fluidity of the granules as indices, we optimized the formulation of Apium graveolens L. capsules by mono-factor test, with the mono-factors including microcrystalline cellulose, aerosil and lactose. In the optimized formula, the contents of aerosil, microcrystalline cellulose and polyvinylpolypyrrolidone were 26%, 30% and 2%, respectively. The aerosil had a satisfactory adsorption for volatile oil, which is important to the viscosity, moldability and fluidity of the granules. Three batches of samples were made using the optimized formula,and the quality evaluation tests showed that mass variation, the moisture content and contents of flavonoids and phthalides all met the quality control criteria. Conclusion The granules of capsules prepared in this study have satisfactory moldability and fluidity.The preparation technique is simple and the quality can be controlled, making it suitable for industrial production.
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Objective To elucidate potential activities of phthalides and terpenoids from Angelica sinensis by theoreticaldocking calculation.Methods Eleven components of phthalides and terpenoids were selected as ligand.Thecrystalline structures of targets related to common diseases were used as the receptors for calculation.Thecalculations were conducted with Schr(o)dinger software package.The grading standard of selectivity was developedaccording to G-score between ligands and receptors.Results Selective targets of phthalides and terpenoids wererelated to nevous system diseases,cancer,pain,diabetes,cardiovascular disease,liver cirrhosis,nephrotic syndrome,inflammatory diseases,rheumatoid arthritis,dermatosis,leukemia,microbial inflections,immune diseases,andhypercholesterolemia.In addition to the medical treatments reported in the literature,our research also indicated thatthese two classes of compounds may be used for tumor,diabetes,rheumatoid arthritis,dermatosis,leukemia,livercirrhosis,and nephrotic syndrome.According to our research,the effects of phthalides and terpenoids may be not sostrong.Conclusion The effects of phthalides and terpenoids on diseases founded through virtual evaluation accord greatly with those reported in experiment and clinic.The combination of computer-aided drug evaluation technique and experiment is definitely an important and fast way to investigate the effects and mechanisms of traditional Chinese medicine.