ABSTRACT
Prunellae Spica is the dried spica of Prunella vulgaris belonging to Labiatae and it is widely used in pharmaceutical and general health fields. As a traditional Chinese medicine cultivated on a large scale, it produces a large amount of non-medicinal parts, which are discarded because they are not effectively used. To analyze the chemical constituents in the different samples from spica, seed, stem, and leaf of P. vulgaris, and explore the application value and development prospect of these parts, this study used ultrahigh performance liquid chromatography-tandem quadrupoles time of flight mass spectrometry(UPLC-Q-TOF-MS/MS) to detect chemical constituents in different parts of P. vulgaris. As a result, 117 compounds were detected. Among them, 87 compounds were identified, including 32 phenolic acids, 8 flavonoids, and 45 triterpenoid saponins. Some new triterpenoid saponins containing the sugar chain with 4-6 sugar units were found. Further, multivariate statistical analysis was conducted on BPI chromatographic peaks of multiple batches of different parts, and the results showed that spica had the most abundant chemical constituents, including salviaflaside and linolenic acid highly contained in the seed and phenolic acids, flavonoids, and triterpenoid saponins in the stem and leaf. In general, the constituents in the spica were composed of those in the seed, stem, and leaf. UPLC was used to determine the content of 6 phenolic acids(danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, salviaflaside, and rosmarinic acid) in different parts. The content of other phenolic acids in the seed was generally lower than that in the spica except that of salviaflaside. The content of salviaflaside in the spica was higher than that in the stem and leaf, but the content of other phenolic acids in the spica was not significantly different from that in the stem. The content of protocatechuic aldehyde and caffeic acid in the spica was lower than that in the leaf. DPPH free radical scavenging method was used to detect the antioxidant activity of four parts, and there was no significant difference in the antioxidant activity between the spica and the stem and leaf, but that was significantly higher than the seed. Moreover, the antioxidant activity of these parts was correlated with the content of total phenolic acids. Based on the above findings, the stem and leaf of P. vulgaris have potential application value. Considering the traditional medication rule, it is feasible to use the whole plant as a medicine. Alternatively, salviaflaside, occurring in the seed, can be used as a marker compound for the quality evaluation of Prunellae Spica, if only using spica as the medicinal part of P. vulgaris, as described in the Chinese Pharmacopoeia(2020 edition).
Subject(s)
Prunella , Saponins , Triterpenes , Antioxidants/chemistry , Tandem Mass Spectrometry/methods , Prunella/chemistry , Chromatography, High Pressure Liquid/methods , Caffeic Acids , Flavonoids/analysis , Triterpenes/analysis , SugarsABSTRACT
In order to establish the standardized processing technology of the hot water washing of Euodiae Fructus, this study, based on the traditional processing method of hot water washing of Euodiae Fructus recorded in ancient works and modern processing specifications of traditional Chinese medicine decoction pieces, took the yield of decoction pieces and the content of main components as the indicators and optimized the processing conditions by orthogonal test based on the results of single factor investigation. At the same time, electronic tongue technology was used to analyze the change law of the taste index of Euodiae Fructus during the hot water washing. The results of the single factor investigation showed that the content of the main components in Euodiae Fructus showed some regular changes during the processing. Specifically, the content of chlorogenic acid, hyperin, isorhamnetin-3-O-rutinoside, isorhamnetin-3-O-galactoside, and dehydroevodiamine decreased significantly, with average decreases of-23.75%,-27.80%,-14.04%,-14.03%, and-13.11%, respectively. The content of limonin increased significantly with an average increase of 19.83%. The content of evodiamine, rutaecarpine, evocarpine, and dihydroevocarpine showed fluctuating changes and generally increased, with average variation amplitudes of 0.54%,-3.78%, 2.69%, and 5.13%, respectively. The orthogonal test results showed that the optimum processing parameters for the hot water washing of Euodiae Fructus were as follows: washing time of 2 min, the solid-to-liquid ratio of 1â¶10 g·mL~(-1), washing temperature of 80 â, washing once, and drying at 50 â. After the hot water washing processing, the average yield of Euodiae Fructus pieces was 94.80%. The content of limonin, evodiamine, and rutaecarpine was higher than those of raw pro-ducts, and the average transfer rates were 102.56%, 103.15%, and 105.16%, respectively. The content of dehydroevodiamine was lower than that of the raw products, and the average transfer rate was 83.04%. The results of taste analysis showed that the hot water washing could significantly reduce the salty, astringent, and bitter tastes of Euodiae Fructus. This study revealed the influence of the hot water washing on the content of main components and taste of Euodiae Fructus, and the processing technology of the hot water was-hing of Euodiae Fructus established in this study was stable, feasible, and suitable for industrial production, which laid a foundation for clarifying its processing principle and improving the quality standard and clinical application value of decoction pieces.
Subject(s)
Drugs, Chinese Herbal , Limonins , Taste , Technology , Chromatography, High Pressure Liquid/methodsABSTRACT
Rosae Radix et Rhizoma is a herbal medicine in a variety of famous Chinese patent medicines, while the quality standard for this medicine remains to be developed due to the insufficient research on the quality of Rosae Radix et Rhizoma from different sources. Therefore, this study comprehensively analyzed the components in Rosae Radix et Rhizoma of different sources from the aspects of extract, component category content, identification based on thin-lay chromatography, active component content determination, and fingerprint, so as to improve the quality control. The results showed that the content of chemical components varied in the samples of different sources, while there was little difference in the chemical composition among the samples. The content of components in the roots of Rosa laevigata was higher than that in the other two species, and the content of components in the roots was higher than that in the stems. The fingerprints of triterpenoids and non-triterpenoids were established, and the content of five main triterpenoids including multiflorin, rosamultin, myrianthic acid, rosolic acid, and tormentic acid in Rosae Radix et Rhizoma was determined. The results were consistent with those of major component categories. In conclusion, the quality of Rosae Radix et Rhizoma is associated with the plant species, producing area, and medicinal parts. The method established in this study lays a foundation for improving the quality standard of Rosae Radix et Rhizoma and provides data support for the rational use of the stem.
Subject(s)
Drugs, Chinese Herbal , Plants, Medicinal , Drugs, Chinese Herbal/chemistry , Rhizome/chemistry , Plant Roots/chemistry , Quality ControlABSTRACT
With the improvement of living standards and changes in working style, the prevalence of abnormal glucose and lipid metabolism in humans is increasing in modern society. Clinically, the related indicators are often improved by changing the lifestyle and/or taking hypoglycemic and lipid-lowering drugs, but there are no therapeutic drugs for disorders of glucose and lipid metabolism at present. Hepatitis C virus core protein binding protein 6(HCBP6) is a newly discovered target that can regulate triglyceride and cholesterol content according to level oscillations in the body, thereby regulating abnormal glucose and lipid metabolism. Relevant studies have shown that ginsenoside Rh_2 can significantly up-regulate the expression of HCBP6, but there are few studies on the effect of Chinese herbal medicines on HCBP6. Moreover, the three-dimensional structural information of HCBP6 has not been determined and the discovery of potential active components acting on HCBP6 is not rapidly advanced. Therefore, the total saponins of eight Chinese herbal medicines commonly used to regulate abnormal glucose and lipid metabolism were selected as the research objects to observe their effect on the expression of HCBP6. Then, the three-dimensional structure of HCBP6 was predicted, followed by molecular docking with saponins in eight Chinese herbal medicines to quickly find potential active components. The results showed that all total saponins tended to up-regulate HCBP6 mRNA and protein expression, where gypenosides showed the optimum effect on up-regulating HCBP6 mRNA and ginsenosides showed the optimum effect on up-regulating HCBP6 protein expression. Reliable protein structures were obtained after the prediction of protein structures using the Robetta website and the evaluation of the predicted structures by SAVES. The saponins from the website and literature were also collected and docked with the predicted protein, and the saponin components were found to have good binding activity to the HCBP6 protein. The results of the study are expected to provide ideas and methods for the discovery of new drugs from Chinese herbal medicines to regulate glucose and lipid metabolism.
Subject(s)
Drugs, Chinese Herbal , Ginsenosides , Saponins , Humans , Glucose , Lipid Metabolism , Molecular Docking Simulation , Drugs, Chinese Herbal/pharmacology , Proteins , RNA, MessengerABSTRACT
To improve the quality control methods of Poria and develop and utilize its resources fully, alkaline extraction was used in this study to determine the yield and content of alkali-soluble polysaccharides of Poria. The alkali-soluble extracts of Poria were obtained according to the optimum extraction conditions on the basis of single-factor test, and 30 batches of samples were determined. The structure and chemical composition of the alkali-soluble extracts was characterized by high-performance gel permeation chromatography(HPGPC), Fourier transform infrared spectrometry(FT-IR), nuclear magnetic resonance(NMR) spectroscopy and high-performance liquid chromatography(HPLC) with 1-phenyl-3-methyl-5-pyrazolone(PMP-HPLC). The results showed that the content of the alkali-soluble extracts was in the range of 46.98%-73.86%. The main component was ß-(1â3)-glucan, and its molecular mass was about 1.093×10~5. Further, the content of alkali-soluble polysaccharides of Poria was measured by UV-Vis spectrophotometry and HPLC coupled with the evaporative light scattering detector(HPLC-ELSD), and 30 batches of samples were measured. The results indicated that the content of alkali-soluble polysaccharides determined by UV-Vis spectrophotometry was in the range of 73.70%-92.57%, and the content of samples from Hubei province was slightly higher than that from Yunnan province, Anhui province and Hunan province. The content of alkali-soluble polysaccharides determined by HPLC-ELSD was in the range of 51.42%-76.69%, and the samples from Hunan province had slightly higher content than that from the other three provinces. The content determined by UV-Vis spectrophotometry was higher than that by HPLC-ELSD. However, the content determined by HPLC-ELSD was close to that of alkali-soluble extract, which could accurately characterize the content of alkali-soluble polysaccharides in Poria, and the method was simple and repeatable. Therefore, it is recommended that the quantitative analysis method for alkali-soluble extract and alkali-soluble polysaccharides by HPLC-ELSD be used in the quality standards of Poria in Chinese Pharmacopeia.
Subject(s)
Poria , Poria/chemistry , Spectroscopy, Fourier Transform Infrared , China , Polysaccharides/chemistry , Reference Standards , Chromatography, High Pressure Liquid/methodsABSTRACT
Galli Gigerii Endothelium Corneum(GGEC), the dried gizzard membrane of Gallus gallus domesticus is a Chinese medicinal material commonly used for digestion. However, due to the particularity of texture and composition, its active ingre-dients have not been clarified so far, and there is also a lack of quality evaluation indicators. In this study, UPLC-Q-TOF-MS was used to analyze the chemical components from the water extract of GGEC, and ten nucleosides were identified for the first time. HPLC fingerprints of the water extracts of GGEC were established and the content of seven nucleosides was determined. The fingerprint similarities of 40 batches of GGEC samples ranged from 0.765 to 0.959, indicating that there were great differences among the GGEC products processed with different methods. In addition, SPSS 22.0 and SIMCA 14.1 were used for hierarchical cluster analysis(HCA) and principal component analysis(PCA) on the 19 common peaks of the HPLC fingerprints of GGEC, and the 40 batches of samples were divided into three categories: raw GGEC, fried GGEC and vinegar-processed GGEC. Eight differential components in GGEC were marked by orthogonal partial least squares discrimination analysis(OPLS-DA), two of which were adenine and thymine. The results of content determination showed that the total content of the seven nucleosides in raw GGEC, fried GGEC and vinegar-processed GGEC were 182.5-416.8, 205.3-368.7, and 194.2-283.0 µg·g~(-1), respectively. There were significant differences in the content of hypoxanthine, thymine and thymidine among the GGEC products processed with different methods(P<0.05), which were graded in the order of fried GGEC>vinegar-processed GGEC>raw GGEC. This suggested that the content of hypoxanthine, thymine and thymidine tended to increase during the frying process, and the variation range might be related to the degree of heat exposure. The established methods in this study were simple and reproducible, and could be used for qualitative and quantitative analysis of GGEC and its processed pro-ducts. This study also provided reference for the establishment of quality standards of GGEC with chemical components as control index.
Subject(s)
Drugs, Chinese Herbal , Nucleosides , Drugs, Chinese Herbal/chemistry , Chromatography, High Pressure Liquid , Acetic Acid , Thymine , Thymidine , Water , HypoxanthinesABSTRACT
To explore the stability characteristics of ß-nicotinamide mononucleotide(NMN) and provide data support for NMN production, preparation, and related product development, this study established a simple HPLC content determination method for NMN in simple substrate and investigated the degradation behavior, degradation products, and degradation kinetics of NMN under various chemical, physical, and biological conditions. The HPLC method employed a Welch Xtimate AQ-C_(18) column(4.6 mm×250 mm, 5 µm), a detection wavelength of 266 nm, a column temperature of 30 â, a flow rate of 1.0 mL·min~(-1), an injection volume of 5 µL, and a mobile phase consisting of methanol(A) and a 10 mmol·L~(-1) ammonium formate aqueous solution(B) with a gradient elution(0-6.7 min, 0-4% A; 6.7-13 min, 4%-18% A; 13-14.2 min, 18% A; 14.2-15 min, 18%-0 A; 15-22 min, 0 A). This method provided good separation between NMN and potential impurities and degradation products, and had a wide linear range, short analysis time, good durability, high accuracy, an average sample recovery rate of 98.71%, and an RSD of 1.2%. The instrument precision had an RSD of 0.26%, and the linearity within the examined range was excellent(R~2≥0.999 9). This method can be applied for NMN content determination in simple substrate. The degradation process of NMN in aqueous solution followed apparent first-order kinetics, with the degradation rate primarily influenced by high temperature and pH. NMN was more stable in low-temperature, neutral, or weakly acidic/alkaline environments. Strong acids or strong alkalis could accelerate its degradation, and its degradation rate was less affected by pepsin and trypsin. In an aqueous solution at room temperature, it followed the kinetic equation lg C_t=0.005 7t + 4.817 2, with t_(0.9) and t_(1/2) values of 95.58, 860.26 h, respectively. The results suggest that pH and temperature are the main factors affecting the stability of NMN in aqueous solution, and low temperature, moisture protection, and a weakly acidic environment are more conducive to the storage and application of NMN and its products.
Subject(s)
Acids , Nicotinamide Mononucleotide , Nicotinamide Mononucleotide/metabolism , Chromatography, High Pressure Liquid/methods , KineticsABSTRACT
The aim of this study was to compare crocins in the fruit of Gardenia jasminoides and Gardenia jasminoides var. radicans. Acchrom XCharge C_(18) column(4.6 mm×250 mm, 5 µm) was used for separation, with mobile phase of acetonitrile and 0.1% formic acid for gradient elution. The detection wavelength was set at 440 nm with a flow rate of 1.0 mL·min~(-1), and the column temperature was 30 â. The high performance liquid chromatography(HPLC) fingerprint of crocin in Gardenia species was established by testing 20 batches of G. jasminoides and 8 batches of G. jasminoides var. radicans samples from different sources, and UHPLC-ESI-Orbitrap-MS/MS technology and reference substances were used to predict and identify the common peaks. The results showed that 20 common chromatographic peaks from the samples were selected and the structures of 16 common peaks were predicted by mass spectrum. Four common peaks(crocin â , â ¡, â ¢, and â £) were identified by the comparison with reference substances. The content of crocin â , â ¡, â ¢, and â £ was determined simultaneously under the same chromatographic condition, and both the system suitability and the methodological investigation results met the requirements of content determination. The relative similarity of HPLC fingerprint of 28 samples to the reference fingerprint was above 0.98. The results of cluster analysis(CA) showed that G. jasminoides and G. jasminoides var. radicans were separately grouped into one group. In the 20 batches of G. jasminoides, the content of crocin â , â ¡, â £, and â ¢ was between 3.58-9.58, 0.230-1.452, 0.014 5-0.135, and 0.301-1.12 mg·g~(-1), respectively, and the total content was between 4.12-12.25 mg·g~(-1). In the 8 batches of G. jasminoides var. radicans, the content of crocin â , â ¡, â £, and â ¢ was between 5.84-11.48, 0.308-0.898, 0.010 6-0.025 5, and 0.675-1.34 mg·g~(-1), respectively, and the total content was between 6.97-13.72 mg·g~(-1). The existing results showed that there is a certain similarity between G. jasminoides and G. jasminoides var. radicans in the composition of crocin, which needs further proved by more batches of samples. The method established in this paper provides references for the quality control of G. jasminoides, G. jasminoides var. radicans, and related products.
Subject(s)
Gardenia , Carotenoids/analysis , Chromatography, High Pressure Liquid/methods , Fruit/chemistry , Gardenia/chemistry , Tandem Mass SpectrometryABSTRACT
A comprehensive quality control method was established to provide references for quality control and evaluation of substance benchmarks of Danggui Sini Decoction(DSD). The HPLC separation was performed on a Kromasil 100 C-8 column(4.6 mm×250 mm, 5 µm) with acetonitrile(A)-0.05% phosphoric acid in water(B) as mobile phase in a gradient elution mode at the flow rate of 1 mL·min~(-1). The column temperature was 25 â and the detection wavelength was set at 275 nm. Under these conditions, the content of seven components, including paeoniflorin, liquiritin, cinnamic acid, cinnamaldehyde, ammonium glycyrrhetate, ligustilide, and asarinin was simultaneously determined. Under the same chromatographic conditions, the HPLC fingerprint method for analysis of 15 batches of DSD was established. The content determination of aristolochic acid I, using the same test solution as the content determination item, was performed on an ACQUITY UPLC BEH C_(18) column(2.1 mm×50 mm, 1.7 µm) with methanol(A)-water(including 0.1% formic acid and 5 mmol·L~(-1) ammonium formate)(B) as the mobile phase in a gradient elution mode at the flow rate of 0.4 mL·min~(-1) and the column temperature of 40 â by LC-MS/MS. The MS conditions included electrospray ionization(ESI) as an ion source, positive ion ionization, selective reaction monitoring(SRM), the parent ion of 359.3, and the daughter ion of 297.8. The results of the methodological investigation all met the requirements of content determination/fingerprint determination. As a result, the content ranges of paeoniflorin, liquiritin, cinnamic acid, cinnamaldehyde, ammonium glycyrrhetate, ligustilide, and asarinin were 5.419 8-11.267 3, 1.023-3.669 8, 0.145 6-0.444 1, 0.099 1-0.321 9, 3.159 1-7.731 9, 0.146 4-0.471 7, and 0.237 3-0.401 0 mg·g~(-1), respectively. Twenty-two common peaks were selected and 10 of them were identified by the comparison with the reference substances. The fingerprint similarity of 15 batches of DSD was in the range of 0.91-0.996 and the content of aristolochic acid I in DSD was 300.03-638.13 ng·g~(-1). The method established in this study is reliable and easy to operate and has great practical value, which can be used for overall quality control of substance benchmarks for DSD.
Subject(s)
Ammonium Compounds , Drugs, Chinese Herbal , Benchmarking , Chromatography, High Pressure Liquid/methods , Chromatography, Liquid , Drugs, Chinese Herbal/chemistry , Quality Control , Tandem Mass Spectrometry/methods , WaterABSTRACT
This study aimed to explore the correlation of the content of 15 non-crocin components of Gardeniae Fructus with its external properties(shape and color). The fruit shape was quantified according to the length/diameter measured by ruler and vernier calliper and the chromaticity values L~*, a~*, b~*, and ΔE~* of all samples were determined by chroma meter. Chromatographic separation was conducted on a Welch Ultimate XB C_(18) column(4.6 mm×250 mm, 5 µm) under gradient elution with acetonitrile solution(A) and 0.1% formic acid aqueous solution(B) as the mobile phase at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 â and the detection wavelength was 238 nm. The high-performance liquid chromatography(HPLC) method was established for simultaneous determination of the content of eight iridoid glycosides, six phenolic acids, and one flavonoid in 21 batches of Gardeniae Fructus samples. The correlation of the content of the 15 components with shapes and chromaticity values in each sample was analyzed by multivariate statistical analysis. According to the circulation situation and traditional experience, 21 batches of Gardeniae Fructus samples were divided into three categories, namely 14 batches of Jiangxi products(small and round, red and yellow), 4 batches of Fujian products(oval, red) and 3 batches of Shuizhizi(Gardenia jasminoides, longest, reddest). The Gardeniae Fructus samples were sequenced as Jiangxi products(1.71) < Fujian products(1.99) < Shuizhizi(2.55) in terms of the length/diameter average, Jiangxi products(17.7) < Fujian products(19.7) ≈ Shuizhizi(19.6) in terms of average value of a~*(red and green), Jiangxi products(24.4) > Fujian products(19.2) ≈ Shuizhizi(19.3) in terms of b~*(yellow and blue), and Jiangxi products(49.8) > Fujian products(48.0) ≈ Shuizhizi(47.8) in terms of L~*(brightness). The total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Jiangxi products was in the ranges of 65.53-99.64, 52.15-89.16, 6.10-11.83, and 0.145-1.81 mg·g~(-1), respectively. The total amount of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin in Fujian products was in the ranges of 69.33-94.35, 63.52-85.19, 5.39-8.41, and 0.333-0.757 mg·g~(-1), respectively. In Shuizhizi, the total content of the 15 components, 8 iridoid glycosides, 6 phenolic acids, and rutin was in the ranges of 77.35-85.98, 68.69-76.56, 7.30-9.05, and 0.368-0.697 mg·g~(-1), respectively. Pearson correlation analysis revealed that Gardeniae Fructus with leaner and longer fruit shape possessed lower content of total phenolic acids(the sum of the six phenolic acids) and rutin, but the correlation with iridoid glycosides was not high. Additionally, the higher content of total phenolic acids and rutin denoted the yellow coloration of Gardeniae Fructus, and the higher content of cryptochlorogenic acid, chlorogenic acid, and rutin meant the brighter color of Gardeniae Fructus. However, the higher content of geniposide and neochlorogenic acid and the lower content of deacetyl asperulosidic acid methyl ester led to the red coloration of Gardeniae Fructus. The results indicated that the morphological characters of Gardeniae Fructus were closely related to its chemical components. The more round shape and the yellower color reflected the higher content of phenolic acids and flavonoid, and Gardeniae Fructus with redder color had higher content of geniposide. OPLA-DA showed that the length/diameter and the content of six iridoid glycosides(gardoside, shanzhiside, gardenoside, genipin 1-gentiobioside, 6ß-hydroxy geniposide, and deacetyl asperulosidic acid methyl ester), two phenolic acids(neochlorogenic acid and cryptochlorogenic acid) and rutin could be used as markers to distinguish three types of samples. This study provided experimental data for the scientific connotation of "quality evaluation through morphological identification" of Gardeniae Fructus.
Subject(s)
Drugs, Chinese Herbal , Gardenia , Chromatography, High Pressure Liquid/methods , Drugs, Chinese Herbal/analysis , Esters/analysis , Flavonoids/analysis , Fruit/chemistry , Gardenia/chemistry , Iridoids/analysis , Rutin/analysisABSTRACT
The purpose of this paper is to establish the HPLC fingerprint and content determination method for Crataegus pinnatifida seeds. The separation was developed on a Welch Ultimate XB C_(18) column(4.6 mm×250 mm, 5 µm) by gradient elution with acetonitrile-water containing 0.1% formic acid as the mobile phase at the flow rate of 1 mL·min~(-1), the column temperature of 30 â, the injection volume of 10 µL, and the detection wavelength of 320 nm. Eighteen batches of samples were analyzed under the above chromatographic conditions to establish the fingerprint of C. pinnatifida seeds from different producing areas and a total of 24 common peaks were selected. The structures of three main chromatographic peaks were identified by comparison to reference substances, and the three compounds were simultaneously analyzed for content determination. They were identified as erythro-(7S,8R)-guaiacylglycerol-ß-coniferyl aldehyde ether, threo-(7R,8R)-guaiacylglycerol-ß-coniferyl aldehyde ether, and balanophonin, respectively. The relative similarity of fingerprints of 18 batches of samples and references ranged from 0.928 to 0.999, and the content of the three compounds was 0.055 1-0.182 7, 0.061 8-0.225 8, and 0.156 8-0.405 6 mg·g~(-1), respectively. SPSS 17.0 and SIMCA 14.1 were used for cluster analysis, principal component analysis(PCA), and orthogonal partial least squares discriminant analysis(OPLS-DA) on the common peaks of the HPLC fingerprint of C. pinnatifida seeds. The results showed that there were significant differences between the two batches of samples from Liaoning province and the other samples, and the three compounds to be tested were the main components leading to the difference of C. pinnatifida seeds. The established method was simple and reliable and can be used for qualitative and quantitative analysis of C. pinnatifida seeds. The findings of this study are expected to provide a scientific basis for quality control of C. pinnatifida seeds.
Subject(s)
Crataegus , Drugs, Chinese Herbal , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal/chemistry , Ethers , Seeds/chemistryABSTRACT
The fruits of Gardenia jasminoides Ellis are an important herb medicine in Traditional Chinese Medicine (TCM) and have been used for thousands of years for clearing away heat and toxic materials. It mainly contains iridoids, pigments, organic acids, and flavonoids. Although belonging to one species, it has two kinds of cultivars and one variety widely distributed and sold. This study aims to develop an integrated and efficient analytical strategy for comprehensive profiling of phytochemicals and clarify the differences in all three populations. Based on reversed-phase ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC/ESI-QTOFMS), an optimized analytical approach for comprehensive profiling of phytochemicals in the fruits of G. jasminoides was established in negative ionization mode. The holistic metabolites profiling was carried out on UHPLC/ESI-QTOFMS and data analysis program Progenesis QI, and a total of 80 metabolites were obtained and interpreted by chromatographic and tandem mass spectral data. The interpretation of metabolites comprises iridoids, pigments, organic acids, and flavonoids. Principal component analysis and partial least square-discriminant analysis were performed, and 19 main different components could be obtained to distinguish the three populations. Combined with non-targeted and targeted data analysis, the integrated strategy developed in this study was feasibly applied to discern differences in the profiles of the phytochemicals accumulating in the fruits of three populations of G. jasminoides.
Subject(s)
Gardenia , Chromatography, High Pressure Liquid/methods , Chromatography, Liquid , Coloring Agents/analysis , Flavonoids/analysis , Fruit/chemistry , Gardenia/chemistry , Iridoids/chemistry , Phytochemicals/analysis , Spectrometry, Mass, Electrospray Ionization/methodsABSTRACT
Polygalae Radix has long been used in China for calming the mind, promoting intelligence, communicating the heart and kidney, eliminating phlegm, and reducing swelling. At present, it is used to treat amnesia, insomnia, and malaise. Modern research has revealed that Polygalae Radix mainly contains triterpenoid saponins, xanthone, oligosaccharide esters, etc., with the activities of improving memory, resisting dementia, protecting the brain, relieving cough, and removing phlegm, as well as sedation and hypnosis. The present study reviews the research progress on chemical composition, pharmacological action, quality control, and metabolism of Polygalae Radix in the past 30 years, to provide a theoretical basis for further research and development.
Subject(s)
Drugs, Chinese Herbal , Polygala , Oligosaccharides , Plant Roots , Quality ControlABSTRACT
A HPLC method was established for simultaneous determination of two organic acids(chlorogenic acid and ferulic acid) and five phthalides(senkyunolide I, senkyunolide H, senkyunolide A, ligustilide, and butylidenephthalide) in Angelicae Sinensis Radix and its processed products to clarify the underlying material transferring rules. The analysis was performed on a Welch Ultimate C_8 column(4.6 mm×250 mm, 5 µm) with acetonitrile(A)-0.085% phosphoric acid water(B) as the mobile phase in a gradient elution mode at the flow rate of 1.1 mL·min~(-1), the column temperature of 25 â, the detection wavelength of 280 nm, and the injection volume of 10 µL. Under these conditions, the content of the above-mentioned seven components was analyzed in 15 batches of Angelicae Sinensis Radix and its processed products, and the transfer rate of each compound was calculated. As a result, in the processed products, the average content of chlorogenic acid was slightly decreased and that of ferulic acid was equivalent to the medicinal materials. The content of senkyunolide I, senkyunolide H, senkyunolide A, and butylidenephthalide showed an increasing trend in the processed products as compared with the medicinal materials. The mass fraction of ligustilide in the medicinal materials was above 0.7%(0.94% on average), meeting the requirement of 0.6% in the Hong Kong Chinese Materia Medica Standards, but was 0.47% on average in the processed products, which was decreased by 50% approximately. Further investigation showed that the content of ligustilide in freshly made processed products of Angelicae Sinensis Radix did not change significantly compared with that in the medicinal materials, indicating that the loss of ligustilide in the processed products mainly occurred in the storage. Therefore, Angelicae Sinensis Radix is suitable for storing in the form of medicinal materials and the freshly made processed products should be used except for special cases. Additionally, it is recommended to control the content of volatile oils or ligustilide in medicinal materials and processed products of Angelicae Sinensis Radix to ensure its effectiveness in clinical medication.
Subject(s)
Angelica sinensis , Drugs, Chinese Herbal , Chlorogenic Acid , Chromatography, High Pressure Liquid , Plant RootsABSTRACT
Based on the textual research on literature, the key information of Wenjing Decoction were tested and identified, and 15 batches of lyophilized powder samples of Wenjing Decoction were prepared. The specific components, including paeoniflorin, glycyrrhizin, ginsenosides(Rg_1, Re and Rb_1), glycyrrhizic acid, and paeonol, were used as indexes to establish the HPLC method for quantitative evaluation, and the content ranges and transfer rates of these components were determined. The results showed that the contents of paeoniflorin, glycyrrhizin, ginsenosides Rg_1 + Re, ginsenoside Rb_1, glycyrrhizic acid, and paeonol in the 15 batches of samples were 0.62%-0.86%, 0.25%-0.76%, 0.14%-0.30%, 0.07%-0.21%, 0.63%-1.16%, and 0.09%-0.25%, respectively, and their transfer rates from the decoction pieces to the reference materials were 14.99%-19.42%, 28.11%-40.93%, 25.92%-61.88%, 25.03%-64.06%, 23.43%-35.53%, and 5.34%-10.44%, respectively. The consistency of the transfer rates between batches indicated that the preparation process was stable. It is suggested that the contents of paeoniflorin, glycyrrhizin, ginsenosides Rg_1 + Re, ginsenoside Rb_1, glycyrrhizic acid, and paeonol in Wenjing Decoction should not be less than 0.52%, 0.35%, 0.15%, 0.10%, 0.63%, and 0.12%, respectively. In this study, we determined the contents and analyzed the quantity transfer process of the index components in Wenjing Decoction, which can provide a basis for the follow-up development of Wenjing Decoction and the quality control of related preparations.
Subject(s)
Drugs, Chinese Herbal , Chromatography, High Pressure Liquid , Glycyrrhizic Acid , Powders , Quality ControlABSTRACT
To obtain the chemical profile of Tibetan medicinal plant â³Banggaâ³, the present study established the HPLC fingerprint of â³Banggaâ³ and inferred common chemical constituents of its two original plants, Aconitum tanguticum and A. naviculare by LC-MS. The HPLC analysis was performed on a Kromasil 100 C_8 column(4.6 mm×250 mm, 5 µm) with acetonitrile(A)-0.1% formic acid in water(B) as mobile phase in a gradient elution mode. Besides, the flow rate was set at 1 mL·min~(-1) and the column temperature was 35 â. The detection wavelength was set at 255 nm and the injection volume was 10 µL. Seventeen batches of â³Banggaâ³ samples were analyzed and the HPLC fingerprint was established under the above conditions. Similarity evaluation was performed using Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(2012). As a result, 16 common peaks were selec-ted and the similarity values of 17 batches of â³Banggaâ³ were in the range of 0.702-0.966. Furthermore, one batch of A. tanguticum and one batch of A. naviculare were analyzed by LC-MS/MS and 74 common compounds were inferred, including 10 phenolic acids, 26 flavonoids, and 38 alkaloids. The established method, with good separation and strong specificity, is simple and feasible, and can be used for the quality control of â³Banggaâ³ and identification of its two original plants. A. tanguticum and A. naviculare are similar in chemical composition and component content, but are quite different in the content of flavonoids.
Subject(s)
Drugs, Chinese Herbal , Plants, Medicinal , Chromatography, High Pressure Liquid , Chromatography, Liquid , Tandem Mass Spectrometry , TibetABSTRACT
The dried fruit body of Phylloporia ribis(Hymenochaetaceae), which prefers to live on the stumps of Lonicera japonica(Caprifoliaceae), has a variety of activities, whereas its pharmacodynamic material basis is not completely clear and there are few reports on its quality control and evaluation. In this study, an UPLC-Q-TOF-MS method was used to analyze the nucleosides and nucleobases in P. ribis and a HPLC method was established for simultaneous determination of 10 nucleosides and nucleobases. MS and MS/MS data were acquired in positive ion mode. Based on the data comparison of the sample and the reference substance, the literature data and the compound databases of ChemSpider and PubChem, 18 nucleosides and nucleobases were identified qualitatively from the water extract of P. ribis for the first time. After optimization, the HPLC was performed using a Welch Ultimate AQ C_(18) column(4.6 mm×250 mm, 5 µm) by gradient elution with acetonitrile and water as mobile phase, the flow rate of 1.0 mL·min~(-1), the detection wavelength of 260 nm, and the column temperature of 30 â. Through the investigation of the extraction method, solvent and time, it was determined that the test solution should be obtained by cold water extraction for 18 h. At the present HPLC conditions, 10 components of uracil, cytidine, hypoxanthine, uridine, thymine, inosine, guanosine, 2'-deoxyinosine, 2'-deoxyguanosine and thymidine could be well separated(R > 1.5) and showed good linearity(r > 0.999 9) in the concentration ranges of 0.247-24.7, 0.283-28.3, 0.273-27.3, 0.256-25.6, 0.257-25.7, 0.318-31.8, 0.245-24.5, 0.267-26.7, 0.250-25.0 and 0.267-26.7 mg·L~(-1), respectively. The average reco-veries of 10 components were 95.78%-104.5%, and the RSDs were 2.2%-5.2%(n=6). The contents of 10 nucleosides and nucleobases in different samples of P. ribis varied greatly, which were 0.021-0.122, 0.004-0.029, 0.014-0.226, 0.009-0.442, 0.003-0.014, 0.002-0.146, 0.007-0.098, 0-0.054, 0.005-0.069, 0.004-0.081 and 0.072-1.28 mg·g~(-1) for uracil, cytidine, hypoxanthine, uridine, thymine, inosine, guanosine, 2'-deoxyinosine, 2'-deoxyguanosine, thymidine and total 10 components, respectively. These results demonstrated that the components had significant differences in the internal quality, and good quality control was needed to ensure the medical efficacy. This study provides a scientific basis for the discovery of pharmacodynamic ingredients, quality control and evaluation of P. ribis.
Subject(s)
Nucleosides , Tandem Mass Spectrometry , Basidiomycota , Chromatography, High Pressure Liquid , GuanosineABSTRACT
This paper aims to solve the problems of complicated-unstable test solution preparation process and insufficient extraction of the active ingredient astragaloside â £ in the legal method for the determination of astragaloside â £ in Astragali Radix. The continuous single-factor analysis of seven main factors affecting the content of astragaloside â £ was carried out by HPLC-ELSD, and then the pre-paration method of test solution was optimized. This optimized method exhibited excellent performance in precision, repeatability and stability. The average recovery rate of astragaloside â £ was 99.65% with RSD 2.2%. Astragaloside â £ showed a good linearity between the logarithm of peak area and the logarithm of injection quantity in the range of 0.46-9.1 µg(r=0.999 6). The contents of astragaloside â £ in 29 batches of Astragali Radix were determined by the new and the legal methods. The results showed that the average content of astragaloside â £ in these Astragali Radix samples determined by the former method was 1.458 times than that of the latter one, indicating the new method was simple, reliable and more adequate to extract target compound. According to the results, it is suggested to improve the content standard of astragaloside â £ in Astragali Radix in the new edition of Chinese Pharmacopeia.
Subject(s)
Astragalus Plant , Drugs, Chinese Herbal , Saponins , Triterpenes , Chromatography, High Pressure Liquid , Triterpenes/analysisABSTRACT
Chrysanthemum is widely used as a type of edible flower and also considered as the important materials of many beverages in China. Due to the occurrence of diseases and pests, and the lack of regulations for species, frequency, dose of pesticides in Chrysanthemum, pesticides have become one of the main pollutants in Chrysanthemum. The pesticide residues in Chrysanthemum were detected frequently and worth noting. This paper focused on the types of pesticides, pesticide residue detection techniques, and risk assessment methods for Chrysanthemums on the basis of relevant literatures. The pesticide residues of traditional Chinese medicine are mainly organochlorines, organophosphorus and pyrethroids, and the detection techniques include gas chromatography(GC), liquid chromatography(LC) or both combined with mass spectrometry(MS). With the increasing use of traditional Chinese medicine, Chrysanthemum is widely circulated in the market. Therefore, it is important to understand the current situation of pesticide residues in different varieties of Chrysanthemum, so as to provide theoretical reference for the control of quality and safety of Chrysanthemum and the formulation of the maximum residue limit.
Subject(s)
Chrysanthemum , Pesticide Residues , China , Chromatography, Liquid , Chrysanthemum/genetics , Gas Chromatography-Mass Spectrometry , Pesticide Residues/analysisABSTRACT
In this paper, the newly isolated tannins were sorted after a review of the literature concerning tannins in recent 10 years, and their research progress was summarized in terms of extraction, isolation, pharmacological activity and metabolism. Hydrolysable tannins and condensed tannins are the main structural types. Modern research shows that tannins have many pharmacological effects, such as bacteriostasis, antioxidation, antitumor, antivirus and blood glucose reduction, and have broad development prospects. They are usually extracted by water, ethanol and acetone and isolated and purified by macroporous resin and gel column chromatography. The packings commonly adopted for the column chromatography mainly included Sephadex LH-20, Diaion HP-20, MCI-gel CHP-20 and Toyopearl HW-40. Modern analytical techniques such as nuclear magnetic resonance spectroscopy(NMR), fast atom bombardment mass spectrometry(FAB-MS) and circular dichroism(CD) are generally used for the structural identification of tannins. Howe-ver, their isolation, purification and structural identification are still challenging. It is necessary to use a variety of high-throughput screening methods to explore their pharmacological activities and to explore the material basis responsible for their functions through experiments in vivo.