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1.
China Journal of Chinese Materia Medica ; (24): 114-125, 2023.
Article in Chinese | WPRIM | ID: wpr-970507

ABSTRACT

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)
Nucleosides , Drugs, Chinese Herbal/chemistry , Chromatography, High Pressure Liquid , Acetic Acid , Thymine , Thymidine , Water , Hypoxanthines
2.
China Journal of Chinese Materia Medica ; (24): 443-454, 2023.
Article in Chinese | WPRIM | ID: wpr-970481

ABSTRACT

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 β-(1→3)-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/chemistry , Spectroscopy, Fourier Transform Infrared , China , Polysaccharides/chemistry , Reference Standards , Chromatography, High Pressure Liquid/methods
3.
China Journal of Chinese Materia Medica ; (24): 3485-3497, 2023.
Article in Chinese | WPRIM | ID: wpr-981499

ABSTRACT

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 1∶10 g·mL~(-1), washing temperature of 80 ℃, washing once, and drying at 50 ℃. 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 , Taste , Limonins , Technology , Chromatography, High Pressure Liquid/methods
4.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 27-37, 2022.
Article in Chinese | WPRIM | ID: wpr-940583

ABSTRACT

ObjectiveTo provide references for the selection of Zingiberis Rhizoma Recens on the research of famous classical formulas and the reasonable uses for medicines and foods through herbal textural research and quality analysis of Zingiberis Rhizoma Recens from main producing areas in China. MethodBy consulting the ancient and modern literature, the name, origin, producing areas, harvest time, processing methods of Zingiberis Rhizoma Recens were summarized. According to the 2020 edition of Chinese Pharmacopoeia, the contents of 6-gingerol, 8-gingerol, 10-gingerol, and volatile oil in Zingiberis Rhizoma Recens samples were determined. ResultHerbal textural research indicated that medicinal Zingiberis Rhizoma Recens originated from the fresh rhizome of Zingiber officinale. Before Tang dynasty, Zingiberis Rhizoma Recens produced in Sichuan was the best. In the Song dynasty, Zingiberis Rhizoma Recens produced in Sichuan, Zhejiang, and Anhui was of excellent quality. The cultivation of Zingiberis Rhizoma Recens in Shandong developed during the Ming and Qing dynasties. From ancient times to the present, the harvest period extended from the autumnal equinox to the winter solstice. Quality evaluation standards of Zingiberis Rhizoma Recens were essentially the same in ancient and present documents, as those with little gluten or gluten-free and strong pungency were preferred. After determination, the contents of 6-gingerol, 8-gingerol, and 10-gingerol in 44 samples were qualified in 27 samples, with a qualified rate of 61.4%. Among them, 17 samples were unqualified in the total contents of 8-gingerol and 10-gingerol. Among these qualified samples, the content of 6-gingerol ranged from 0.067% to 0.255%, and the total contents of 8-gingerol and 10-gingerol ranged from 0.040% to 0.131%. The content of volatile oil in 36 samples were qualified in 33 samples, with a qualified rate of 91.7%. Among the qualified samples, the content of volatile oil ranged from 0.175% to 0.410%. ConclusionZingiberis Rhizoma Recens has been used as medicines and foods since ancient times, and the genuine producing areas are consistent in ancient and present times, while the quality of the products, especially the medicinal Zingiberis Rhizoma Recens, should be monitored. Medicinal Zingiberis Rhizoma Recens planted in Leshan city of Sichuan province contains high contents of effective components, followed by Qujing and Wenshan cities of Yunnan province. Zingiberis Rhizoma Recens planted in Shandong and other places is mostly edible.

5.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 181-193, 2022.
Article in Chinese | WPRIM | ID: wpr-940533

ABSTRACT

Wuzhuyu Tang (WZYT), a classical traditional Chinese medicine (TCM) formula, was first recorded in Treatise on Cold Damage by the prestigious physician ZHANG Zhong-jing in the Eastern Han Dynasty, and included in Catalogue of Ancient Classical Formulas (First Batch). WZYT is composed of four medcinals: Euodiae Fructus, Ginseng Radix et Rhizoma, Zingiberis Rhizoma Recens, and Jujubae Fructus, which has the effects of warming the middle and tonifying deficiency, dissipating cold and descending adverse qi. Based on data mining, this paper analyzes the modern clinical research literature on WZYT, which is expected to lay a basis for clarifying the "disease-symptom-prescription-medicinal" relationship of WZYT, as well as its modern clinical indications and clinical dosage. With the search term "Wuzhuyu Tang", 253 complete medical records were retrieved from CNKI, VIP, and Wanfang (2000-2020), involving 292 TCM prescriptions. Microsoft Excel 2019 was employed to establish the medical record database and the main clinical indications were statistically analyzed. Moreover, the syndromes, incidence law, and medication regularity were summed up. The result indicates WZYT has a wide range of modern clinical applications, mainly including the treatment of headache, dizziness, vomiting, diarrhea, dysmenorrhea, morning sickness, and other diseases, and the "deficiency, cold, and reversal" symptoms, mainly manifested as nausea and vomiting, headache, fatigue and lack of strength, reversal cold of hands and feet, poor appetite, gloomy complexion, dizziness, aversion to wind and cold, abdominal pain, sloppy diarrhea, abdominal distension, poor sleep, pale tongue, white coating, and deep thread wiry pulse. These diseases and symptoms mainly occur in women and middle-aged people. In most cases, medicinals are added or subtracted according to the symptoms, and the common doses of Euodiae Fructus, Zingiberis Rhizoma Recens, Codonopsis Radix or Ginseng Radix et Rhizoma, and Jujubae Fructus in the original prescription are 6-15 g, 10-15 g, 10-15 g or 9-12 g, and 4-6, respectively. The added medicinals are in the descending order of Pinelliae Rhizoma, Atractylodis Macrocephalae Rhizoma, Poria, Glycyrrhize Radix et Rhizoma, and Chuanxiong Rhizoma according to the frequency.

6.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 212-217, 2022.
Article in Chinese | WPRIM | ID: wpr-940307

ABSTRACT

In this paper, the key technical problems in the research and development of famous classical formulas are analyzed. Firstly, the puzzled problem for a long-time, which is conversion relationship from medicinal metrology of Han dynasty (HD) to that of modern (gram,g), is comprehensively expounded that one Liang (两) of HD=3 g is more appropriate. Secondly, the model and principles of quality consistency evaluation are given for the transformation from the quality of authoritative basic sample prepared by casserole (ABS-C) to the quality consistency in Laboratory process, pilot-scale process and industrial production. The consistency evaluation model is ξABS-X=K1(Q1ABS-X/Q1ABS-C)+K2(Q2ABS-X/Q2ABS-C)+……+Ki(QiABS-X/QiABS-C)=∑Ki(QiABS-X/QiABS-C)(i=1,2,3……n). In the formula, ABS-X means laboratory reference sample ABS-C (ABS-L), pilot-scale ABS-C (ABS-mP) or industrial production ABS-C (ABS-P), ξABS-X means the quality consistency rate or similarity degree of ABS-L, ABS-mP and ABS-P processes with ABS-C, Ki means the weight of each quality evaluation index (i), QiABS-X is the data of i in ABS-L, ABS-mP, ABS-P samples, and QiABS-C is the data (or mean) of i in ABS-C sample. Thirdly, in order to control the quality of the herbal medicines whose active ingredients were unknown, their chemical constituents should be studied deeply, and if necessary, the bioassay research should be carried out according to the main efficacy or indication of famous classical formulas. Finally, for the special processing of some herbal medicines, it is difficult to formulate the processing method, technology and standard of prepared slices. It is suggested that the scientific connotation and historical evolution of the special processing method should be thoroughly sorted out, and its technological characteristics are summarized, the modern processing technology and production processes are simulated, and then the corresponding processing methods and quality standards are formulated.

7.
China Journal of Chinese Materia Medica ; (24): 391-397, 2021.
Article in Chinese | WPRIM | ID: wpr-878986

ABSTRACT

This paper aims to solve the problems of complicated-unstable test solution preparation process and insufficient extraction of the active ingredient astragaloside Ⅳ in the legal method for the determination of astragaloside Ⅳ in Astragali Radix. The continuous single-factor analysis of seven main factors affecting the content of astragaloside Ⅳ 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 Ⅳ was 99.65% with RSD 2.2%. Astragaloside Ⅳ 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 Ⅳ in 29 batches of Astragali Radix were determined by the new and the legal methods. The results showed that the average content of astragaloside Ⅳ 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 Ⅳ in Astragali Radix in the new edition of Chinese Pharmacopeia.


Subject(s)
Astragalus Plant , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Saponins , Triterpenes/analysis
8.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 113-126, 2021.
Article in Chinese | WPRIM | ID: wpr-906524

ABSTRACT

Objective:To analyze the chemical constituents in Euodiae Fructus by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS). Method:The chromatographic separation was performed on an ACQUITY UPLC BEH C<sub>18</sub> column (2.1 mm×100 mm, 1.7 μm) with acetonitrile (A)-0.1% formic acid aqueous solution (B) as mobile phase (0-3 min, 6%A; 3-4 min, 6%-10%A; 4-7 min, 10%-12%A; 7-8 min, 12%-14%A; 8-13 min, 14%-15%A; 13-15 min, 15%-20%A; 15-18 min, 20%-30%A; 18-21 min, 30%-49%A; 21-25 min, 49%-51%A; 25-27 min, 51%-73%A; 27-30 min, 73%-80%A; 30-31 min, 80%-100%A; 31-32 min, 100%A) for gradient elution. The column temperature was 35 ℃, and the flow rate was 0.4 mL·min<sup>-1</sup>. Mass spectrometry was performed using an electrospray ionization and data were collected in positive and negative ion modes, and the detection range was <italic>m</italic>/<italic>z</italic> 100-1 200. The chemical constituents in Euodiae Fructus were identified rapidly and comprehensively based on the accurate relative molecular mass and combined with literature data and reference substances. Result:A total of 92 chemical constituents were speculatively identified from the 70% methanol extract of Euodiae Fructus, including 39 alkaloids, 19 flavonoids, 12 limonoids, 20 phenolic acids and 2 organic acids. Among them, 26 compounds were confirmed by the reference substances. Conclusion:The compound types of Euodiae Fructus are multiple and quite different in polarity. The chemical compositions of Euodiae Fructus from different regions and species are similar. The established method is rapid and accurate, with which the chemical compositions of Euodiae Fructus have been identified comprehensively. Therefore, this study provides an experimental reference for further clarifying active and toxic constituents of Euodiae Fructus.

9.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 138-145, 2021.
Article in Chinese | WPRIM | ID: wpr-906217

ABSTRACT

Objective:Through comprehensive evaluation and analysis of the quality of Liuwei Dihuang (LWDH) preparations from different manufacturers and combining factors such as production technology, the key factors in the quality control of LWDH preparations are explored to provide a reference for improving the quality control level of LWDH preparations. Method:Morroniside, loganin and paeonol as quality control markers of LWDH products were determined by high performance liquid chromatography (HPLC), the mobile phase was acetonitrile (A) -0.3% phosphoric acid aqueous solution (B) for gradient elution (0-5 min, 5%-8%A; 5-20 min, 8%A; 20-35 min, 8%-20%A; 35-45 min, 20%-60%A; 45-55 min, 60%A), the detection wavelength of paeonol was at 274 nm, and the detection wavelengths of morroniside and loganin were at 240 nm. The quality characteristics of LWDH preparations with different dosage forms (big candied pills, water-honeyed pills, concentrated pills, hard capsules and soft capsules) from different manufacturers were analyzed. Combined these results with their actual production processes, the key-points of quality control in the whole production process were discussed. Result:The contents of three index ingredients in 128 batches of LWDH preparations were all in conformity with the standards of the 2015 edition of <italic>Chinese Pharmacopoeia</italic>, however, the content limit of some dosage forms in the current standard was unreasonable. For example, although the daily dose of crude drugs for big candied pills were almost twice the dose of water- honeyed pills (15.00, 8.57 g, respectively), they got exactly the same daily limits of the contents for both the quality markers. What′s more, these two formulations had the same process, so the differences between the process obviously could not be the reason of these differences. Conclusion:It is recommended that for the products with different dosage forms should have a similar content limits, if there are no obvious distinctions between their production processes. Which may benefit the quality control of the products with multi-dosage forms. The research on the quality standards of proprietary Chinese medicines should deeply study the existing characteristics of the quality standards, and fully respect the laws of the quality attributes of traditional Chinese medicines and the rules of the production process of Chinese patent medicines.

10.
China Journal of Chinese Materia Medica ; (24): 4051-4060, 2021.
Article in Chinese | WPRIM | ID: wpr-888062

ABSTRACT

This research established the HPLC methods for the determination of perillaketone, perillaldehyde, caffeic acid, scutellarin, and rosmarinic acid in 33 batches of Perillae Folium. Kromasil C_(18)(4.6 × 250 mm, 5 μm) chromatographic column was used, and the mobile phase for determination of the perillaketone and perillaldehyde was methanol-water(55∶45) solution, at a flow rate of 1.0 mL·min~(-1), with the column temperature at 30 ℃. The mobile phase for the determination of caffeic acid, scutellarin and rosmarinic acid was methanol(A)-0.2% phosphoric acid aqueous solution(B) with gradient elution(0-20 min, 25%-30% A; 20-60 min, 30%-43% A). The flow rate was 1.0 mL·min~(-1) and the column temperature was set at 30 ℃. The results showed that the established method can achieve good separation of the five components in samples, with a good linear relationship and high accuracy, indicating that the methods can be used for the determination of Perillae Folium. The results showed that all samples contained five components. And the content of rosmarinic acid(0.04%-1.57%) > scutellarin(0.03%-0.77%) > perillaldehyde(0.02%-0.66%) > perillaketone(0.03%-0.30%) > caffeic acid(0.006%-0.07%). Thirty-three Batches of Perillae Folium can be grouped into 5 categories. There are certain content rules and region specificities under different clusters. Perillaketone, perillaldehyde, and rosmarinic acid can be used as the main markers to evaluate the quality of Perillae Folium.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Plant Extracts , Plant Leaves
11.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 145-153, 2020.
Article in Chinese | WPRIM | ID: wpr-873166

ABSTRACT

Objective:To study the water soluble chemical constituents in rhizoma of Acorus tatarinowii and transformation pathway of nucleosides in the process of water extraction. Method:Compounds were isolated and purified by column chromatography on macroporous resin,Sephadex LH-20,ODS and preparative HPLC. Their structures were identified on the basis of physicochemical properties and spectral data. Nucleosides were identified from aqueous extract of A. tatarinowii,and their stability was investigated by HPLC. The possible transformation pathways of nucleosides in aqueous extract of A. tatarinowii were studied by nucleotide addition test. Result:Eleven compounds including four nucleosides,four phenylpropanoids,two alkaloids and a furfural were isolated,and identified as uridine(1),adenine(2),guanosine(3),adenosine(4),5-hydroxymethylfurfural(5),5-(hydroxymethyl)-1H-pyrrole-2-carboxaldehyde(6),(threo)1',2'-dihydroxyasarone(7),(erythro)1',2'-dihydroxyasarone(8),acoraminol A(9),acoraminol B(10),and tatarine A(11). The chromatographic peaks of compounds 1-4 and cytidine were identified from aqueous extract of A. tatarinowii by HPLC. After ultrasonic extraction for 0.5 h,the stability of nucleosides in water was poor. After ultrasonic extraction for 3 h or refluxing extraction for 0.5 h,the stability of nucleosides in water was good. Four transformation pathways including 5'-cytidylic acid→cytidine,uridine monophosphate→uridine,guanosine monophosphate,guanosine and adenosine-5'-monophosphate,adenosine 5'-diphosphate,adenosine 5'-triphosphorate,adenosine,adenine might exist in water extract of A. tatarinowii. Conclusion:Compounds 1-4 and 6 were isolated from the genus Acorus for the first time. These compounds further enriched the chemical constituents of A. tatarinowii. The stability and transformation pathway of nucleosides in A. tatarinowii provides reference data for the analysis of nucleosides in A. tatarinowii and other traditional Chinese medicine.

12.
China Journal of Chinese Materia Medica ; (24): 1371-1380, 2019.
Article in Chinese | WPRIM | ID: wpr-774546

ABSTRACT

HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃ and the injection volume was 20 μL. The experimental data were analyzed by the SPSS 22.0 and GraphPad Prism 7.0. The established triterpenoids fingerprints were specific, and the 10 components were well separated and showed good linearity(r≥0.999 6) within the concentration ranges tested. The mean recoveries were between 98.53%-103.8%(RSD 1.7%-2.7%). The method was specific and repeatable, and could be used for identification and quality evaluation of Poria. The results showed that the contents of 10 triterpenoids were positively correlated with each other. The contents of 10 triterpenoids of samples collected from producing areas were higher than that collected from markets. The total contents of 10 triterpenoids of samples collected from Hubei and Yunnan province were slightly higher than that from Anhui province, but the contents of samples from Anhui province were varied in smaller ranges.


Subject(s)
China , Chromatography, High Pressure Liquid , Materia Medica , Poria , Chemistry
13.
China Journal of Chinese Materia Medica ; (24): 730-739, 2019.
Article in Chinese | WPRIM | ID: wpr-777501

ABSTRACT

To solve the problems of the poor resolution of chromatographic separation,the weak durability of the relative correction factors,and the low accuracy of content determination results in the quantitative analysis of multi-components by single-marker( QAMS) method with andrographolide as the internal reference substance in the existing research of Andrographis Herba,a new QAMS method using dehydroandrographolide as the internal reference substance was established for the first time in this study. This new method can be used to simultaneously determine four diterpene lactones,including andrographolide( A),neoandrographolide( B),14-deoxyandrographolide( C),and dehydroandrographolide( S) through the optimization of chromatographic conditions and systematic investigation of methodology. At the present HPLC chromatographic conditions,four components could be well separated( R > 1. 5),and the methodology validations could satisfy the requirement of quantitative analysis. The relative correction factors( RCFs) of fA/S,fB/S,fC/S were determined as 0. 65,0. 54,0. 78,respectively. The relative standard deviations( RSDs) of their RCFs ranged between 1. 3%-5. 1%,0. 25%-0. 33%,0. 070%-0. 15%,0. 070%-0. 22%,respectively with three brands of HPLC instruments,five brands of C18 column,different flow rates( 0. 9,1. 0,1. 1 m L·min~(-1)),and different column temperatures( 25,30,35 ℃),indicating good durability of the RCFs. The relative retention value( RRV) method was used to locate the chromatographic peak of the components to be determined.The RRVs of rA/S,rB/S,and rC/Swere 0. 44,0. 86,0. 97,respectively. The RSDs of the RRVs ranged between 0. 030%-1. 6% with different HPLC instruments and columns,showing accurate peak location. The present QAMS method and the external standard method( ESM)were both used to determine the contents of four diterpene lactones from Andrographis Herba( 6 batches of medicinal materials and 18 batches of cut crude drugs). The relative errors of the determined content results between two methods were less than 2. 0%. It demonstrated that there was no significant difference in content results between these two methods,indicating good accuracy of the present QAMS method. Therefore,in this study,an accurate and highly durable QAMS method using dehydroandrographolide as the internal reference substance was established for simultaneous determination of four diterpene lactones. This method could be used to effectively control the quality of Andrographis Herba and provide technical basis for the formulation of traditional Chinese medicine industry standard and improvement of the Chinese Pharmacopoeia standard of Andrographis Herba.


Subject(s)
Andrographis , Chromatography, High Pressure Liquid , Diterpenes , Drugs, Chinese Herbal , Quality Control
14.
Acta Pharmaceutica Sinica ; (12): 1157-1164, 2017.
Article in Chinese | WPRIM | ID: wpr-779708

ABSTRACT

An ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF/MS)method has been established to analyze the bioactive components of the aqueous extract of Euodiae Fructusand detect the metabolites in rats after oral administration of the aqueous extract. Compounds were detected by analyzing their retention times, high resolution mass data, mass spectra and comparing with the reference substances. As a result, 27 compounds were characterized from the aqueous extract of Euodiae Fructus, and 25 compounds were identified on the basis of the reference substances. 16 parent compounds and 35 metabolites were detected in rats' plasma, urine and feces samples, and all of the parent compounds were determined unambiguously through comparison with the reference substances. Four classes of compounds were identified from the aqueous extract of Euodiae Fructus, including phenolic acids, limonins, flavonoid glycosides and alkaloids. Phenolic acids, flavonoid glycosides and alkaloids were detected in rats' plasma, urine and feces, while limonins were detected in the urine and feces. The main metabolism pathways of these compounds in rats might include hydroxyl, hydrogenation, methylation, sulfating, glucuronidation, and so on. The results of this study provide references in the material basis of Euodiae Fructus in vivo.

15.
China Journal of Chinese Materia Medica ; (24): 1819-1824, 2017.
Article in Chinese | WPRIM | ID: wpr-256089

ABSTRACT

As an outstanding representative of traditional Chinese medicine(TCM) prescriptions accumulated from famous TCM doctors' clinical experiences in past dynasties, classical TCM excellent prescriptions (cTCMeP) are the most valuable part of TCM system. To support the research and development of cTCMeP, a series of regulations and measures were issued to encourage its simplified registration. There is still a long-way to go because many key problems and puzzles about technology, registration and administration in cTCMeP R&D process are not resolved. Based on the analysis of registration and management regulations of botanical drug products in FDA of USA and Japan, and EMA of Europe, the possible key problems and countermeasures in chemistry, manufacture and control (CMC) of simplified registration of cTCMeP were analyzed on the consideration of its actual situation. The method of "reference decoction extract by traditional prescription" (RDETP) was firstly proposed as standard to evaluate the quality and preparation uniformity between the new developing product under simplified registration and traditional original usages of cTCMeP, instead of Standard Decoction method in Japan. "Totality of the evidence" approach, mass balance and bioassay/biological assay of cTCMeP were emphatically suggested to introduce to the quality uniformity evaluation system in the raw drug material, drug substance and final product between the modern product and traditional decoction.

16.
China Journal of Chinese Materia Medica ; (24): 2144-2148, 2016.
Article in Chinese | WPRIM | ID: wpr-236057

ABSTRACT

Everted intestinal sac models were used to investigate the intestinal absorption of the 4 alkaloids(berberine, palmatine, coptisine, and epiberberine) in Fuzheng Xiaozheng Fang(FZ) at different intestine segments. The absorption parameters of each component were calculated; SPSS 20.0 software was used to analyze the data and evaluate the absorption characteristics at different intestinal segments. The results showed that all the four active ingredients conformed to zero-order absorption rate. There was significant difference in absorption rate constant (Ka) between the four ingredients at low dose and medium and high dose groups(P<0.05), but there was no significant difference in Ka between medium dose and high dose. The absorption mechanization of four ingredients presented two absorption manners: positive diffusion and passive absorption. The absorptive amount of 4 alkaloids in ileum was slightly greater than that of jejunum, but no significant differences were observed, which indicated that these four alkaloids had no specific absorption windows in intestinal segment.

17.
China Journal of Chinese Materia Medica ; (24): 1865-1871, 2015.
Article in Chinese | WPRIM | ID: wpr-351248

ABSTRACT

The methods to determine the total phenols, total saponins, and marker constituents salidroside, chlorogenic acid and 3, 4-dihydroxy-phenylethyl-β-D-glucopyranoside in the samples of Sargentodoxae Caulis were established to provide the evidence for the improvement and revision of the quality standard of the crude material recorded in the Chinese Pharmacopoeia (2015 Edition). The content of total phenols was determined by ultraviolet spectrophotometry, using gallic acid as a reference substance. The content of total saponins was determined by ultraviolet spectrophotometry, using 3-O-[β-D-xylopyranosyl-(1-2)-O-β-D-glucuronopyranosyl]-28-O-[β-D-glucopyranosyl] asiatic acid as a reference substance. The contents of salidroside, chlorogenic acid and 3,4-dihydroxy-phenylethyl-β-D-glucopyranoside were detected by HPLC. The linear ranges were 1.01-7.04 mg x L(-1) for total phenols, 37.7-201 μg for total saponins, 0.025 8-1.55 μg for salidroside, 0.076 2-5.44 μg for chlorogenic acid, and 0.064 9-3.47 μg for 3,4-dihydroxy-phenylethyl-βP-D-glucopyranoside, respectively. Their average recoveries were 99.12%, 99.11% 105.5%, 99.08%, and 101.6%, respectively. The contents of total phenols and total saponins were 3. 04% -11. 9% and 0. 87% -3. 63%. The contents of salidroside, chlorogenic acid and 3,4-dihydroxy-phenylethyl-β-D-glucopyranoside fluctuated from 0.018% to 0. 572%, from 0.041% to 1.75% and from 0.035% to 1.32%. The established methods were reproducible, and they could be used for the quality control of Sargentodoxae Caulis. The present investigation suggested that total phenols, salidroside, and chlorogenic acid should be recorded in the quality standard of Sargentodoxae Caulis and their contents should not be less than 6.8% for total phenols, 0.040% for salidroside, and 0.21% for chlorogenic acid.


Subject(s)
China , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Magnoliopsida , Chemistry , Phenol , Plant Stems , Chemistry , Saponins , Triterpenes
18.
China Journal of Chinese Materia Medica ; (24): 1877-1886, 2015.
Article in Chinese | WPRIM | ID: wpr-351246

ABSTRACT

To establish quality standards of Euonymus fortunei, and supply scientific evidence for the quality control of Euonymus fortunei. Empirical and microscopic identification methods were adopted to observe morphological and histological characters. The contents of water, total ash, acid-insoluble ash and alcohol-soluble extractive were analysed according to the methods of Chinese Pharmaco- poeia (2010). Dulcitol and reference herbs were used to identify materia medica of Euonymus fortunei by TLC method. The total flavonol glycosides contents were analysed by HPLC method, using quercetin and kaempferol as reference substances. Quercetin and kaempferol were separated on a C18 column (4.6 mm x 250 mm, 5 μm) with methanol-0.1% formic acid(51:49) as the mobile phase and detected at 366 nm. The flavonoid aglycones content was then multiplied by a conversion coefficient, and the result was the total flavonol glycosides content. The macroscopical identification, microscopic features and TLC methods were proper. The average contents of water, total ash, acid-insoluble ash, alcohol-soluble extractive and total flavonol glycosides were 8.76%, 6.48%, 0.31%, 17.48% and 0.211% , respectively. The quality standards established on the basis of the research results were suitable for the quality evaluation of Euonymus fortunei.


Subject(s)
China , Chromatography, High Pressure Liquid , Chromatography, Thin Layer , Drugs, Chinese Herbal , Chemistry , Reference Standards , Euonymus , Chemistry , Mass Spectrometry , Quality Control
19.
China Journal of Chinese Materia Medica ; (24): 1826-1833, 2014.
Article in Chinese | WPRIM | ID: wpr-327912

ABSTRACT

<p><b>OBJECTIVE</b>To study the technical feasibility of QAMS to determine different structural types of ingredients in Zhizi Jinhua pill, a Chinese patent medicine.</p><p><b>METHOD</b>Emodin was chosen as the internal reference substance. The relative correction factors (RCF) of berberine, baicalin, wogonoside, baicalein, aloe-emodin, wogonin, rhein, chrysophanol and physcion to emodin were calculated with the peak areas determined at 254 nm. The ruggedness of these RCFs was validated. The contents of emodin in the samples of Zhizi Jinhua pill were determined by using the external standard method, and the contents of the other nine ingredients were calculated by their RCFs. The contents of these ten ingredients in all samples were also determined by the external standard method.</p><p><b>RESULT</b>No significant differences were observed between the quantitative results of the two methods. The obtained RCFs were credible.</p><p><b>CONCLUSION</b>The established QAMS method can be used for quantitative determination of different structural types of multi-compounds in Zhizi Jinhua pill. It can provide reference for the quality control of Chinese patent medicine.</p>


Subject(s)
Chromatography, High Pressure Liquid , Methods , Dosage Forms , Drugs, Chinese Herbal , Chemistry , Quality Control
20.
China Journal of Chinese Materia Medica ; (24): 2693-2698, 2014.
Article in Chinese | WPRIM | ID: wpr-330268

ABSTRACT

This study is to develop a HPLC method for quality evaluation of Euodiae Fructus and related species by simultaneous determination limonin, indole alkaloids (14-fomyldihydroxyrutaecarpine, evodiamine, rutaecarpine), and quinolone alkaloids [1-methyl-2-undecyl-4 (1H)-quinolone, evocarpine, dihydroevocarpine] in the fruits of five Evodia species. Samples were analyzed on a YMC C18 column (4.6 mm x 250 mm, 5 microm) eluted with mobile phases of acetonitrile (A), tetrahydrofuran (B), and a buffer solution of 5 mmol x L(-1) ammonium acetate (pH 3.8) (C) in a linear gradient mode. The column temperature was 30 degrees C and the flow rate was 1.0 mL x min(-1). The PDA detector wavelengths were set at 220 and 250 nm. The seven compounds were well separated and showed good linearity (r = 0.999 9) within the concentration ranges tested. The mean recoveries were between 96.7%-102.4% (RSD 1.4%-3.1%). Through the validation, the method was proved to be accurate and repeatable. All the seven constituents were detected in the fruits of five species, but the contents of them varied widely in different samples. The total contents of seven constituents in 16 batches of Euodiae Fructus were 9.46-69.9 mg x g(-1), and the mean content was 28.2 mg x g(-1). The total content of seven constituents in E. compacta and E. fargesii was 25.8, 7.69 mg x g(-1), respectively.


Subject(s)
Chromatography, High Pressure Liquid , Methods , Drugs, Chinese Herbal , Chemistry , Evodia , Chemistry , Fruit , Chemistry , Time Factors
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