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Structures of peimissine, verticine, verticinone, imperialine, isoverticine, ebeiedinone, hupehenine and ebeiedine.
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To establish an HPLC-ELSD method for the simultaneous determination of five major bioactive isosteroidal alkaloids and gluco-alkaloids in the bulbs of Fritillaria namely peimissine, imperialine, sinpeinine A, imperialine-3 beta-glucoside and yibeinoside A.
A Nova-Pak C18 column (150 mm x 3.9 mm ID) was used. The chromatography was carried out with...
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Context 1
... author. Tel.: 1852-2609-6824; fax: 1852- Most of the Fritillaria alkaloids ( Fig. 1) are non- 2603-5139. chromophoric, which make the use of direct UV previously reported to analyze the major active and / or chromophore of analytes, ELSD should also Fritillaria alkaloids in Beimu. One reported high- be a suitable detection method for HPLC analysis of performance liquid chromatography (HPLC)-UV Fritillaria alkaloids. ...
Context 2
... UV previously reported to analyze the major active and / or chromophore of analytes, ELSD should also Fritillaria alkaloids in Beimu. One reported high- be a suitable detection method for HPLC analysis of performance liquid chromatography (HPLC)-UV Fritillaria alkaloids. The aim of the present study is method could only determine peimissine ( Fig. 1), a to develop a simple and sensitive direct HPLC Fritillaria alkaloid containing one double bond, at a analytical method using ELSD for the simultaneous very low wavelength at 205 nm [9]. Our research determination of the major biologically active Fritil- team has previously developed both HPLC-UV [11] laria alkaloids in various ...
Citations
... High performance liquid chromatography (HPLC) equipped with various detector is a conventional technique applied to determine the isosteroidal alkaloids in the dried bulbs of Fritillaria, in addition to evaporative light scattering detection (ELSD) [143][144][145][146][147][148][149] and charged aerosol detector [150] used for the sulfur-fumigation process. Nucleosides and nucleobases in Fritillaria bulbs have been mentioned in the above chapters and these components in different Fritillaria species were simultaneously determined by a HPLC diode-array detector (DAD) [151][152][153]. ...
Fritillaria naturally grows in the temperate region of Northern Hemisphere and mainly distributes in Central Asia, Mediterranean region, and North America. The dried bulbs from a dozen species of this genus have been usually used as herbal medicine, named Beimu in China. Beimu had rich sources of phytochemicals and have extensively applied to respiratory diseases including coronavirus disease (COVID-19). Fritillaria species have alkaloids that act as the main active components that contribute multiple biological activities, including anti-tussive, expectorant, and anti-asthmatic effects, especially against certain respiratory diseases. Other compounds (terpenoids, steroidal saponins, and phenylpropanoids) have also been identified in species of Fritillaria . In this review, readers will discover a brief summary of traditional uses and a comprehensive description of the chemical profiles, biological properties, and analytical techniques used for quality control. In general, the detailed summary reveals 293 specialized metabolites that have been isolated and analyzed in Fritillaria species. This review may provide a scientific basis for the chemical ecology and metabolomics in which compound identification of certain species remains a limiting step.
Fritillaria pallidiflora Schrenk has been treasured in traditional classic medicine as an antitussive, antiasthmatic and expectorant for hundreds of years. With gradually decreasing wild F. pallidiflora resources, the herb can no longer satisfy the demand. Artificial cultivation is one of the most effective ways to solve the contradiction between supply and demand in the medicinal material market. During the growth of Rhizomes medicinal plants, root biomass and active ingredient content showed dynamic accumulated variation with increasing cultivation years. Up to now, hardly any attempts have been made to investigate the relationship between quality and cultivation years of F. pallidiflora. Therefore, in this paper, we determined the optimum harvesting time by comparing biomass and biological characteristics of F. pallidiflora at different cultivation times. High-performance liquid chromatography with evaporative light scattering detection and phenol-sulfuric acid visible spectrophotometry was performed to determine imperialine and polysaccharide content of F. pallidiflora bulbs. From year 1 to 6 of cultivation, we observed an upward trend in plant height, diameter and dry weight of F. pallidiflora, while water content decreased. Plant height and dry weight increased remarkably during the fourth year of cultivation. The content of imperialine and polysaccharide of F. pallidiflora bulbs, on the other hand, showed an upward trend from year 1 to 3, after which it decreased from year 3 to 6. By comparing plant growth, biomass development and the accumulation of imperialine and polysaccharide, the best harvesting time of F. pallidiflora was determined to be after 4 years of cultivation. Our results showed that it is possible to establish a “safe, effective, stable and controllable” production process, which could play an important role in achieving sustainable utilization of F. pallidiflora resources.
A simple, sensitive and selective liquid chromatography–tandem mass spectrometry (LC–MS–MS) method was developed for simultaneous quantitation of four isosteroidal alkaloids (peimine, peiminine, peimisine, and delavine) in rat plasma. Carbamazepine was selected as internal standard (IS). The LC–MS–MS system coupled with an electrospray ionization (ESI) source was performed in the multiple reaction monitoring (MRM) mode. The transitions of the isosteroidal alkaloids executed as following: m/z 432.4 → 414.4 for peimine, m/z 430.5 → 412.4 for peiminine, m/z 428.4 → 114.2 for peimisine, m/z 416.5 → 105.2 for delavine, and m/z 237.2 → 194.2 for carbamazepine (IS). Sample preparation was performed with liquid–liquid extraction using ethyl acetate after carbamazepine (IS) spiked. The separation was performed on a Welch C18 column (3.5 μm, 2.1 × 100 mm), and a gradient elution of methanol and 5 mmol L−1 ammonium acetate in 0.1 % formic acid aqueous solution was used. The retention time was less than 8.0 min. Linearity was obtained over the concentration range of 0.2–200 ng mL−1 for peimine and peiminine, and 1.0–200 ng mL−1 for peimisine and delavine. The method was linear for all analytes with correlation coefficients >0.995. The intra-day and inter-day accuracy and precision of the assay were acceptable. This method has been successfully applied to the pharmacokinetic study of Bulbus Fritillariae Cirrhosae extract after oral administration to rats.
A reliable and accurate liquid chromatography with evaporative light scattering detection (LC-ELSD) method was developed for
simultaneous determination of five constituents in Xue-Fu-Zhu-Yu capsule, a widely used prescription of traditional Chinese
medicine (TCM). The chromatographic separation was performed on a Symmetry C18 column (150 mm×4.6 mm, 5.0 μm) using gradient elution of acetonitrile and water (containing 1.0% acetic acid). The flow rate
was 0.6 mL/min and the temperature of column was 30°C. A good linearity correlation was obtained over the investigated concentration
ranges. Recoveries of the five components varied from 97.31% to 99.84% (RSD<4.0%). The validated method was successfully applied
to the quality assessment of Xue-Fu-Zhu-Yu capsule.
Phytochemical Variation in
Fritillaria cirrhosa
D. Don (
Chuan Bei Mu
) in Relation to Plant Reproductive Stage and Timing of Harvest. Economic development in southwest China and the increasing use of traditional Chinese medicine (TCM) worldwide have led to intensified collection of native medicinal plants. Fritillaria cirrhosa D. Don (Chuan Bei Mu), commonly used for the treatment of cough in TCM, is endemic to the Hengduan Mountain region of southwest China and is under increasing pressure from over-collection and decreasing suitable alpine habitat. The bioactive compounds in F. cirrhosa bulbs, isosteroidal alkaloids, are greatly influenced by environmental conditions and fluctuate in content and concentration with plant age and reproductive stage. Aiming at obtaining useful information for the sustainable management of wild F. cirrhosa populations, we evaluated how the phytochemical composition of F. cirrhosa bulbs varies at various stages of plant reproductive development. Using chemical methods and high-performance liquid chromatography, we extracted and analyzed two major bioactive alkaloids from F. cirrhosa bulb samples collected throughout the Hengduan Mountain region. Plant reproductive stage was found to affect the concentration of bioactive alkaloids in F. cirrhosa bulbs. Bulb alkaloid concentration was highest during the early stages of fruit development and decreased significantly with fruit maturation. These results lend biochemical support to the practice of harvesting F. cirrhosa during the early stages of plant senescence (i.e., early fruit development).
A sensitive and reliable HPLC-diode-array detector method was developed for the first time to simultaneously determine nine nucleosides and nucleobases including uracil, cytidine, guanine, uridine, thymine, inosine, guanosine, thymidine and adenosine in 13 different Fritillaria species. The analysis was performed on a BaseLine C18 column with a gradient of acetonitrile in water at a flow rate of 0.8 mL/min. The diode-array detector wavelength was set at 260 nm for the UV detection of nucleosides and nucleobases. Satisfactory separation of these compounds was obtained in less than 40 min. The optimized method provided good linear relation (r(2)>0.9995 for all the investigated analytes), satisfactory precision (RSD <1.51%) and good recovery (from 97.64 to 101.16%). The established method was successfully applied to simultaneous determination of nine nucleosides and nucleobases in 61 batches of samples from 13 Fritillaria species collected from different habitats in China, which could be helpful to control the quality of Fritillaria bulbs.
High-performance liquid chromatography with evaporative light scattering detection (HPLC/ELSD) was established for simultaneous determination of seven major bioactive components of Qingkailing injection including adenosine, geniposide, chlorogenic acid, baicalin, ursodeoxycholic acid, cholic acid, and hyodeoxycholic acid. The proposed method was applied to analyze ten various Qingkailing injections and produced data with acceptable linearity, repeatability, precision and accuracy having a limit of detection (LOD) of 10-50 ng. In comparison with UV detection, HPLC/ELSD permits the determination of non-chromophoric compounds without prior derivatization, and shows good compatibility to the multi-components of complex analytes. The proposed method is a useful alternative for routine analysis in the quality control of traditional Chinese medicine.
An HPLC with evaporative light scattering detection (ELSD) and ESI-MS was established for the simultaneous determination of eight triterpenoids in Radix Achyranthis Bidentatae. The optimal chromatographic conditions were achieved on a Zorbax C18 column by linear gradient elution with 0.08% v/v aqueous formic acid and ACN as the mobile phase at the flow rate of 0.8 mL/min. Temperature for the detector drift tube was set at 101 degrees C and the nitrogen flow rate was 2.8 L/min. The identities of the analytes were accomplished by comparing retention times and mass data with those of reference compounds. The validation of the method included tests of linearity, sensitivity, repeatability, recovery, and stability. All the calibration curves of the eight triterpenoids showed good linear regression (R2 >0.997) within the test ranges. The method provides desirable repeatability with overall intra- and interday variations of less than 4.9%. The obtained recoveries varied between 93.6 and 98.1% while the RSDs were below 3.9% (n = 3). The analysis results indicate that the content of investigated triterpenoids in Radix Achyranthis Bidentatae from different locations was greatly diverse, and the triterpenoids could be used as chemical markers for the discrimination of genuine and ungenuine crude drugs.
Steroidal alkaloids are naturally occurring nitrogen-containing compounds in many edible or medicinal plants, such as potato, tomato, Fritillaria and American hellebore, which possess a variety of toxicological and pharmacological effects on humans. The aim of this study is to explore the potential of liquid chromatography/electrospray ionization time-of-flight mass spectrometry (LC/ESI-TOF-MS) method in the determination of these important alkaloids in plant matrices. The application of this method has been proven through 26 naturally occurring steroidal alkaloids in Fritillaria species. Accurate mass measurements within 4 ppm error were obtained for all the alkaloids detected out of various plant matrices, which allowed an unequivocal identification of the target steroidal alkaloids. The bunching factor for mass spectrometer, an important parameter significantly affecting the precision and accuracy of quantitative method, was firstly optimized in this work and satisfactory precision and linearity were achieved by the optimization of that parameter. The ranges of RSD values of intra-day and inter-day variability for all alkaloids were decreased remarkably from 41.8-159% and 13.2-140% to 0.32-7.98% and 2.37-16.1%, respectively, when the value of bunching factor was optimized from 1 to 3. Linearity of response more than two orders of magnitude was also demonstrated (regression coefficient >0.99). The LC/TOF-MS detection method offered improvements to the sensitivity, compared with previously applied LC (or GC) methods, with limits of detection down to 0.0014-0.0335 microg/ml. The results in this paper illustrate the robustness and applicability of LC/TOF-MS for steroidal alkaloids analysis in plant samples. In addition, relative quantitative determination of steroidal alkaloid with one popular analyte verticinone which is commercially available was also investigated in order to break through the choke point of lack of standards in phytochemical analysis. The accuracies of relative quantitative method for steroidal alkaloids determinations with verticinone were 90.6-110.0% (average 98.5%) suggesting that it is feasible to quantify steroidal alkaloids by the proposed relative quantitative determination method within acceptable errors.
