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Pruni Semen,the seed of several unique Prunus plants,is a traditional purgative herbal material.To determine the authentic sources of Pruni Semen,46 samples from four species were collected and analyzed.Ten compounds including multiflorin A(Mul A),a notable purative compound,were isolated and identified by chemical separation and nuclear magnetic resonance spectroscopy.Seventy-six communal components were identified by ultra-high performance liquid chromatography with linear ion trap-quadrupole Orbitrap mass spectrometry,and acetyl flavonoid glycosides were recognized as characteristic constituents.The flavonoids were distributed in the seed coat and cyanogenic glycosides in the kernel.Based on this,methods for identifying Pruni Semen from different sources were established using chemical fingerprinting,quantitative analysis of the eight principal compounds,hierarchical cluster analysis,principal component analysis,and orthogonal partial least squares discriminant analysis.The results showed that the samples were divided into two categories:one is the small seeds from Prunus humilis(Ph)and Prunus japonica(Pj),and the other is the big seeds from Prunus pedunculata(Pp)and Prunus triloba(Pt).The average content of Mul A was 3.02.6.93,0.40,and 0.29 mg/g,while the average content of amygdalin was 18.5,17.7,31.5,and 30.9 mg/g in Ph,Pj,Pp,and Pt,respectively.All the above information suggests that small seeds might be superior sources of Pruni Semen.This is the first comprehensive report on the identification of chemical components in Pruni Semen from different species.
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OBJECTIVE：To compare the quality between Stamen typhae and pollen of T. angustifolia ，and provide scientific evidence for the improvement of quality standard of T. angustifolia . METHODS ：Fifteen batches of S. typhae were collected. Pollen minus sieve ，impurity plus sieve （filament and anther ）were sift out from S. typhae according to the identification method of T. angustifolia in Chinese Pharmacopoeia （2015 edition）. The characteristics and components of S. typhae and pollen ，filament and anther of T. angustifolia were comfirmed by impurity ， character examination and microscope ， TLC. The contents of isorhamnetin-3-O-neohesperidoside and typhaneoside in S. typhae and pollen ，impurities plus sieve （filament and anther ）of T. angustifolia were determined by HPLC. RESULTS ：S. typhae was a mixture of pollen ，anther and filament of T. angustifolia ，in the form of brownish yellow flocculent. The pollen of S. typhae was yellow powder with delicate hand feel ，slight smell and light taste；the surface of cells was slightly striped. The filaments and anthers were filiform and short-term ，rough and astringent ，and the cell surface were long strip. TLC chromatogram of S. typhae ，pollen and impurity of T. angustifolia had the same color spots at the same location. The contents of isorhamnetin- 3-O-neohesperidoside，typhaneoside and their aggregate were the highest in pollen （0.42％，0.24％，0.64％）；the second in S. typhae （0.22％，0.17％，0.39％）；the lowest in the impurities plus sieve （0.19％， 0.14％，0.33％）. The total contents of isorhamnetin- 3-O-neohesperidoside and typhaneoside in S. typhae and in impurities plus sieve did not reach the content limit stipulated in Chinese Pharmacopoeia （not less than 0.50％）. CONCLUSIONS：The medicinal components of T. angustifolia mainly exist in pollen. It is suggested that S. typhae should be used as the raw material to obtain pollen，and should not be used directly.
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ABSTRACT OBJECTIVE：To evaluate the in vitro and in vivo genotoxicity of emodin-8-O-β-D-glucoside（EG），and to compare the difference of in vitro cell test and in vivo test of rats. METHODS：2D and 3D hepatocyte models were established by in vitro two-dimensional（2D）and three-dimensional（3D）cell culture. After modeling，2D and 3D hepatocyte were divided into blank control group（0.5％ DMSO），mitomycin C group（positive control，0.1 μg/mL），EG low-dose，medium-dose and high-dose groups（10，50，200 μg/mL），respectively. The micronucleus ratio and tail DNA％ of HepaRG cells were detected. SD rats were divided into blank control group（0.5％ sodium carboxymethyl cellulose），ethyl methanesulfonate group（positive control，200 mg/kg），EG low-dose，medium-dose and high-dose groups（100，300，1 000 mg/kg），with 6 rats in each group. They were given medicine intragastrically for consecutive 15 d，once a day. 15 days later，the micronucleus formation rate of bone marrow polychromatic erythrocytes and hepatocytes，the tail DNA％ and tail distance of peripheral blood lymphocytes and hepatocytes were measured. RESULTS：In the in vitro 2D HepaRG hepatocyte model，compared with blank control group，the micronucleus formation rate and tail DNA％ of HepaRG cell were increased significantly in mitomycin C group （P＜0.01）. There was no statistical significance in micronucleus formation rate and tail DNA％ of HepaRG cell among EG groups（P＞0.05）. In 3D HepaRG cell model， compared with blank control group， micronucleus formation rate and tail DNA％ of HepaRG cell were increased significantly in mitomycin C group （P＜0.01 or P＜0.001）， while tail DNA％ of HepaRG cell wasincreased significantly in EG high-dose group（P＜0.01）. In the in vivo test，compared with blank control group，the micronucleus formation rate of bone marrow polychromatic erythrocytes and hepatocytes，the tail DNA％ and tail distance of peripheral blood lymphocytes and hepatocytes were all increased significantly in ethyl methanesulfonate group（P＜0.01）. Tail DNA％ of peripheral blood lymphocytes was increased significantly in EG high-dose group （P＜0.01）. There was no statistical significance in the micronucleus formation rate of bone marrow polychromatic erythrocytes and hepatocytes，the tail DNA％ and tail distance of hepatocytes among EG groups（P＞0.05）；with the increase of dose，there was an increasing trend. CONCLUSIONS：The results of this study suggest that in 2D cell model，EG not lead to chromosome breakage and DNA damage，but the long-term administration and repeated administration in vivo of 3D cell model show that EG has a certain risk of DNA damage，so the evaluation results of 3D HepaRG cell model are more similar to those of rats in vivo. KEYWORDS Emodin-8-O-β-D-glucoside；Genotoxicity；Two-dimensional culture；Three-dimensional culture；Rat；Micronucleus test
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OBJECTIVE： To investigate the status of sulfur fumigation of TCM and its decoction pieces， and to put forward the suggestions on limit standard of sulfur dioxide residue. METHODS： The information of 374 varieties of TCM and sulfur dioxide residue were collected from the provincial and municipal drug inspection institutions of 27 provinces，municipalities and autonomous regions in China during 2013-2017， and then summarized and analyzed. The average value，median value，maximum value，qualification rate and detection rate of sulfur dioxide residue of 121 varieties with the sample number ≥10 batches were classified and statistically analyzed. RESULTS： This investigation involved 374 varieties of TCM and its decoction pieces， and a total of 13 776 batches of samples. The average content of sulfur dioxide was 242 mg/kg，the median value was 27 mg/kg，and the maximum value was 8 782 mg/kg. The overall qualified rate was 79.7％. According to the results of classified statistics， among the 10 varieties whose limit shall not exceed 400 mg/kg，5 varieties，including Codonopsis pilosula， Radix Trichosanthis， Asparagus cochinchinensis， Pueraria lobata， Achyranthes bidentata， were seriously affected by sulfur fumigation，and the qualified rate was less than 80％. Among the varieties with the sample number≥30 batches， there was no or very little abuse of sulfur fumigation in 16 varieties， such as Carthamus tinctorius； 19 varieties， such as Eupolyphaga Steleophaga， had excessive sulfur fumigation， but it was not serious； 25 varieties，such as Lonicera japonica，had severe excessive sulfur fumigation. Among the varieties with the sample number of 10-29 batches，33 varieties including Ziziphus jujube seed had no or very little abuse of sulfur fumigation； 8 varieties including Cuscuta chinensis had excessive sulfur fumigation but were not serious； 10 varieties including Pericarpium Trichosanthis had serious excessive sulfur fumigation. CONCLUSIONS： For the varieties with no or very little excessive sulfur fumigation，it is recommended that batch testing should not be carried out and a single list should be made； for the varieties with sulfur fumigation or severe sulfur fumigation， it is suggested to increase the sulfur dioxide residue limit under all varieties in the 2020 edition of Chinese Pharmacopoeia， and set the limit for the varieties with severe sulfur fumigation to be no more than 400 mg/kg，while the limit for the 2025 edition of Chinese Pharmacopoeia can be reduced to no more than 150 mg/kg. Other varieties should retain the provisions of “sulfur dioxide residue of sulfur dioxide medicinal materials and decoction pieces （except for minerals） shall not exceed 150 mg/kg” in the general rules 0212 “for the identification of medicinal materials and decoction pieces” in the 2015 edition of Chinese Pharmacopoeia （part Ⅳ）.
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OBJECTIVE： To provide reference for perfecting the quality standard revision of TCM preparations in medical institutions， and improving the quality standard of TCM preparations in medical institutions. METHODS： By sorting out the quality standards of TCM preparations in Guangdong provincial medical institution preparation specification， this paper summarized the main problems and put forward suggestions for improvement. RESULTS & CONCLUSIONS： There are 897 kinds of TCM preparations included in the Guangdong provincial medical institution preparation specification. The recent quality standards （2017 edition） have been greatly improved compared with those of the first edition （1985 edition）； however， there are still some problems in the overall quality control of preparations， quantitative control of indicative components， project specificity， source control of medicinal materials， control of medicinal materials not included in the Chinese Pharmacopoeia and quality standards of the same series of varieties. It is suggested that on the premise of considering both advancement and applicability， the quality control of the whole， local and toxic preparations of TCM hospitals should be strengthened， the detection methods with good specificity and reproducibility should be properly updated， the control of key parameters of production process should be strengthened， the quality standard of TCM preparations in medical institutions should be fully improved， so as to provide the products with safe， effective and controllable in quality products in medical institutions.
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OBJECTIVE： To establish a fluorescence identification method of the microscopic characteristics for Plantagin Semen and its adulterants， and to provide technical support for the market supervision and inspection of TCM decoction pieces. METHODS： Under visible and ultraviolet light， comparative study and identification of the Plantagin Semen （seeds of Platago asiatica L. and Platago depressa Willd.） and its adulterants as seeds of Platago major L.， fruits of Schizonepeta tenuifolia Briq.， seeds of Codonopsis pilosula （Franch.） Nannf， seeds （peeled） of Kochia scoparia （L.） Schrad.， fruits of Bupleurum chinense DC. were carried out by means of stereoscopic fluorescence microscopy from aspects of overall surface characteristics， umbilicus characteristics and section characteristics. RESULTS： Under visible light， the surface texture of Plantagin Semen was wavy stripe or fine wrinkle， while the adulterants were wavy stripe， longitudinal edge or texture was not obvious. The umbilicus of Plantagin Semen was located in the center of the ventral surface， while that of adulterants were located at one end except for P. major. In the section of Plantagin Semen， there were obvious direct embryos， in which the adulterants were small or circular embryos except for P. major. Under ultraviolet light， P. asiatica had obvious wavy stripes in surface， orange and light blue-green fluorescence； P. depressa had grid-shaped wrinkles and gray-blue and gray-brown fluorescence； the umbilical fluorescence of Plantagin Semen was strong， and the fluorescence of the adulterants was weak except for S. tenuifolia. There were obvious differences in fluorescence color， embryo size and distribution between the section of Plantagin Semen and adulterants. CONCLUSIONS： The stereoscopic fluorescence microscopy is effect and accurate for the identification of Plantagin Semen.
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Objective To establish limit test method of camphor in Niuhuang qingxin pills (prescription of the bureau) . Methods The separation was performed on an HP-INNOWAX capillary column (0.25 mm×30 m, 0.25 μm) and the column temperature was 110 ℃ . The temperatures of the inlet and the FID detector were 200 and 230 ℃ , respectively. The flow rate of the carrier gas was 1.8 mL·min-1 and the split ratio was 10:1. The injection volume was 1 μL. Results Good linearity was obtained for camphor within the range of 1.65 to 165 μg·mL-1, and the average recovery of low, medium, high concentration were 99.12％, 99.56％ and 99.56％, respectively,with RSD were 1.01％,0.69％ and 0.38％, respectively. Trace camphor was found in 7 samples out of 38 samples from 9 manufactures. Conclusion The proposed method was accurate, sensitive and simple, and was suitable for quality evaluation and safety control of Niuhuang qingxin pills (prescription of the bureau) .
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Objective: To establish a GC method for the determination of borneol and isoborneol in Niuhuang Qingxin pills ( pre-scription of the bureau). Methods: A capillary column HP-INNOWAX(30 m×0. 25 mm,0. 25 μm) was used and the column tem-perature was kept at 110 ℃. The temperature of the inlet and the FID was 200 ℃ and 230 ℃, respectively. The carrier gas was N2 and the flow rate of the carrier gas was 1. 8 ml·min-1. The split ratio was 10: 1, and the injection volume was 1 μl. Results: The linear response range of borneol and isoborneol was 0. 01-5. 09 μg·ml-1(r=0. 999 5) and 0. 01-5. 03 μg·ml-1(r=0. 999 1), re-spectively. And the average recovery was 99. 34% and 99. 24% with the RSD of 0. 59% and 0. 62% , respectively (n=6). Conclu-sion: The proposed method is accurate, sensitive and simple, and can be used for the quality control of Niuhuang Qingxin pills (pre-scription of the bureau).
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Chinese medicinal materials occupy an important position in China's health industry. However, its overall quality needs to be improved and it is in urgent need of regulation. Exploring the formation of effective organizational mechanisms and industry models has become an urgent need of the industry. In this context, the alliance of coconstruction and sharing Chinese herbal medicine base came into being. The alliance is based on the pursuit of the quality of Chinese herbal medicines and continues to promote the construction of Chinese herbal medicines. The Alliance provides a platform for economic and scientific cooperation in the industry. Its purpose is to guide the promotion of the standardization of local varieties and the construction of modern Chinese medicine agricultural enterprises based on the development needs of Chinese herbal medicine resources and the common interests of all members. As an important content, we will strive to expand the new pattern of coordinated development of traditional Chinese medicine agriculture and industry, explore the establishment of a new organizational system for modern Chinese medicine agricultural production with controllable quality, output and price under the link of production and demand. For the sustainable, stable and healthy development of the Chinese medicine industry, it will serve 1.3 billion people and serve humanity, provide high-quality sustainable Chinese herbal medicine resources. Since its establishment six years ago, the alliance has carried out work on key aspects such as standardized production of Chinese herbal medicines, plant protection, decoction processing, supply and demand docking, medicinal materials standards, poverty alleviation, breeding, and provided technical support to enterprises. During this period, the alliance also proposed the concept of"three-no and one- all"requires the members to take the lead in achieving the standards of"sulfur- free processing, no aflatoxin pollution, pollution-free, traceable throughout the whole", setting a benchmark for the industry.
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Objective:To determine residual sulfite in traditional Chinese medicinal materials or pieces processed by sulfur fumi-gation respectively by iodine titration, acid-base titration and ion chromatography and compare the results. Methods:The three meth-ods were used to determine four kinds of Chinese herbal medicines including Codonopsis radix, Dioscoreae rhizoma, Achyranthis bident-atae Radix and Atractulodis Macrocephalae Rhizoma, the recovery tests were also performed and the results were analyzed and compared to summarize the characteristics and quality control requirements of each method. Results:Iodine titration and acid-base titration had the advantages of simple operation process and low cost. However, there were many interference factors in the two methods, and due to different principles, they were suitable for the determination of different varieties of herbal medicines. Ion chromatography method had the advantages of high sensitivity and strong specificity, while the cost was high. Conclusion: It is suggested that proper methods should be chosen for the determination of sulfur dioxide residues according to actual situations.
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<p><b>OBJECTIVE</b>To establish an HPLC method to simultaneously determine six ingredients in zedoary turmeric oil and its related injections.</p><p><b>METHOD</b>HPLC analysis was performed on Waters Symmetry C18 (4.6 mm x 250 mm, 5 microm). The mobile phase was composed of methanol and water solution in gradient elution mode with at a flow rate of 1.0 mL x min(-1). The column temperature was 30 degrees C and the UV detection wavelength was 215 nm.</p><p><b>RESULT</b>The six ingredients were separated well. The linear ranges of curdione, curcumol, germacrone, curzerene, furanodiene and beta-elemene were 1.74-347.00, 2.38-475.00, 2.49-497.00, 2.07-826.00, 5.05-1009.00, 4.78-955.00 mg x L(-1) (r > or = 0.9996), respectively. The average recoveries were above 95% (RSD <3.0%, n=9).</p><p><b>CONCLUSION</b>The method is accurate, reliable and reproducible, it can be used for the quality control of zedoary turmeric oil and its related injections.</p>
Subject(s)
Chromatography, High Pressure Liquid , Methods , Curcuma , Chemistry , Injections , Oils, VolatileABSTRACT
Cuiru oral liquid (COL ) for the promotion of lactation is prepared from an aqueous extract of Angelica sinensis, Astragalus membranaceus (Fisch.) Bge., Rehmbnnia glutinosa Libosch.,et al. Its formulatiou and processing were briefly desctibed, and the quality standard and stability of the finished product were studied. Results showed that the formu lation processing and stability of COL were suitable for clinical trial. Moreover, its pharmacology was briefly described.
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Objective To study the chemical constituents of Helicia nilagirica. Methods The ethanol extract was seperated by petroleum ether, dichloromethane, and n-butanol in sequence, then isolated by silica gel column chromatography. The structures were identified and elucidated by physicochemical pro-(perties) and spectral analysis. Results Four compounds were isolated from the petroleum ether extract and identified as n-hexadecane acid (Ⅰ), ?-sitosterol (Ⅱ), ?-sitosterol-3-O-?-D-glucoside-6′-acetate (Ⅲ), and daucosterol (Ⅳ). Conclusion All the compounds are isolated from the plant for the first time. Compounds Ⅰ, Ⅲ, Ⅳ are isolated from the plants of Helicia Lour. for the first time, and compound Ⅲ is a new natural product.
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Object To study the chemical constituents of the whole plant of Selaginella stauntoniana Spring. Methods Various chromatographic techniques were employed for the isolation and purification of its constituents, and structurally identified by spectral analysis (IR, UV, MS, 1HNMR, 13CNMR) and chemical evidence. Results Four compounds were identified from its extract as: emodin (Ⅰ), ginkgetin (Ⅱ), hinokiflavone (Ⅲ), amentoflavone (Ⅳ). Conclusion All the compounds were isolated in this plant for the first time; compound Ⅰ was found from the plants of Selaginellaceae Beauv. for the first time.