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1.
Molecules ; 28(3)2023 Jan 20.
Article in English | MEDLINE | ID: mdl-36770712

ABSTRACT

The tuberous root of Ophiopogon japonicus (Thunb.) Ker-Gawl. is a well-known Chinese medicine also called Maidong (MD) in Chinese. It could be divided into "Chuanmaidong" (CMD) and "Zhemaidong" (ZMD), according to the geographic origins. Meanwhile, the root of Liriope spicata (Thunb.) Lour. var. prolifera Y. T. Ma (SMD) is occasionally used as a substitute for MD in the market. In this study, a reliable pressurized liquid extraction and HPLC-DAD-ELSD method was developed for the simultaneous determination of nine chemical components, including four steroidal saponins (ophiopojaponin C, ophiopogonin D, liriopesides B and ophiopogonin D'), four homoisoflavonoids (methylophiopogonone A, methylophiopogonone B, methylophiopogonanone A and methylophiopogonanone B) and one sapogenin (ruscogenin) in CMD, ZMD and SMD. The method was validated in terms of linearity, sensitivity, precision, repeatability and accuracy, and then applied to the real samples from different origins. The results indicated that there were significant differences in the contents of the investigated compounds in CMD, ZMD and SMD. Ruscogenin was not detected in all the samples, and liriopesides B was only found in SMD samples. CMD contained higher ophiopogonin D and ophiopogonin D', while the other compounds were more abundant in ZMD. Moreover, the anticancer effects of the herbal extracts and selected components against A2780 human ovarian cancer cells were also compared. CMD and ZMD showed similar cytotoxic effects, which were stronger than those of SMD. The effects of MD may be due to the significant anticancer potential of ophiopognin D' and homoisoflavonoids. These results suggested that there were great differences in the chemical composition and pharmacological activity among CMD, ZMD and SMD; thus, their origins should be carefully considered in clinical application.


Subject(s)
Drugs, Chinese Herbal , Ophiopogon , Ovarian Neoplasms , Saponins , Spiro Compounds , Humans , Female , Ophiopogon/chemistry , Cell Line, Tumor , Saponins/pharmacology , Saponins/chemistry , Drugs, Chinese Herbal/chemistry
2.
Molecules ; 27(21)2022 Oct 30.
Article in English | MEDLINE | ID: mdl-36364204

ABSTRACT

Zhejiang Ophiopogonjaponicus (ZOJ) is a specific variety of Ophiopogon japonicus with characteristic steroidal saponins and homoisoflavonoids, which are also main pharmacodynamic constituents with clinical effects, including curing inflammation and cardiovascular diseases. However, few analysis methods were applied to simultaneously and quantitatively determine two kinds of its constituents, and hazardous organic solvents are mostly used for extraction. In this study, a new validated simultaneous extraction and determination method for four characteristic steroidal saponins and homoisoflavonoids in ZOJ was established by ionic liquid-ultrasonic extraction (IL-UAE) combined with HPLC-DAD-ELSD analysis, which can be used for the quality control of ZOJ. Chromatographic separation was performed with a DAD wavelength at 296 nm, and the ELSD parameters of the drift tube temperature (DTT), atomizer temperature (AT), and nitrogen gas pressure (NGP) were set at 20% heating power, 70 °C, and 25 psi, respectively. The optimal IL-UAE conditions were 1 mol/L [Bmim]CF3SO3 aqueous solution, a liquid-material ratio of 40 mL/g, and an ultrasonic time of 60 min. The proposed method is reliable, reproducible, and accurate, which were verified with real sample assays. Consequently, this work will be helpful for the quality control of ZOJ. It can also present a promising reference for the simultaneous extraction and determination of different kinds of constituents in other medicinal plants.


Subject(s)
Drugs, Chinese Herbal , Ophiopogon , Saponins , Ophiopogon/chemistry , Drugs, Chinese Herbal/chemistry , Saponins/chemistry , Chromatography, High Pressure Liquid/methods
3.
Phytochem Anal ; 33(1): 5-11, 2022 Jan.
Article in English | MEDLINE | ID: mdl-34275160

ABSTRACT

OBJECTIVES: Because the purity of the two impurities reference standard (RS) of cefathiamidine is not easy to obtain, HPLC-PDA-ELSD were used to determin the RRFs of cefathiamidine impurities. METHODS: Peak area correction was applied to calculate RRFs to eliminate the influence of different responses caused by the difference in pH between the two mobile phases of HPLC-PDA and HPLC-PDA-ELSD. The resulting RRF values have been verified by qNMR. CONCLUSION: The new calcution method described in this article provides a reliable research idea for determintion the RRFs by HPLC-PDA-ELSD, especially when the purity of RS is unknown and the mobile phase of HPLC-PDA and HPLC-PDA-ELSD have difference. This method can be mutually verified with qNMR to ensure the accuracy of RRFs. It is also promingsing replace determination RRF by qNMR becausing economical, simple and low cost.


Subject(s)
Light , Chromatography, High Pressure Liquid , Scattering, Radiation
4.
J Agric Food Chem ; 69(38): 11485-11493, 2021 Sep 29.
Article in English | MEDLINE | ID: mdl-34547203

ABSTRACT

Food matrices consist of many components with different physical and chemical properties that may influence instrumental robustness. The soybean contains fatty coextractives which may have a deleterious effect on the gas chromatography (GC) system. In this study, the efficiencies of PSA, C18OH, C18, silica, aluminum oxide, and Florisil, as dSPE clean-up sorbents, were evaluated by the high-performance liquid chromatography (HPLC) diode-array detector and evaporative light-scattering detector analysis. The dithiocarbamates in soybean samples are determined as CS2 using acidic hydrolysis and isooctane partitioning, followed by GC-PFPD and GC-ITD-MS analyses. The linearity of the analytical curves, the instrument limit of detection matrix effects, the trueness and precision, and the method limit of quantification (LOQ) were assessed in the validation study. Milled soybean was spiked with thiram solution at three concentration levels (corresponding to 0.05, 0.1, and 0.5 mg CS2 kg-1) for recovery determination. Silica appeared to be an effective and cheap sorbent to remove coextracted matrix components without causing any CS2 losses. Recoveries were in the range of 68-91%, with relative standard deviations ≤ 8.7%. The method LOQ was 0.05 mg CS2 kg-1, and both GC-ITD-MS and GC-PFPD systems appeared to be appropriate and complementary to determine dithiocarbamate residues in soybean extracts.


Subject(s)
Fungicides, Industrial , Pesticide Residues , Chromatography, Gas , Chromatography, High Pressure Liquid , Pesticide Residues/analysis , Solid Phase Extraction , Glycine max
5.
J Sci Food Agric ; 101(4): 1491-1498, 2021 Mar 15.
Article in English | MEDLINE | ID: mdl-32844459

ABSTRACT

BACKGROUND: The present study aimed to explore the chemical characteristics of mountainous forest cultivated ginseng (MFCG) and garden ginseng (GG) with respect to their ginsenosides and oligosaccharides. METHODS: A high-performance liquid chromatography with diode-array detection-evaporative light-scattering detection technique was adopted to investigate the ginseosides and oligosaccharides of GG and MFCG. RESULTS: The features of ginsenosides showed Rg1/Re in different parts of GG and MFCG: main root > lateral root > fibrous root, as well as Rg1/Re in the main root: MFCG > GG, indicating that the Rg1/Re is related to age of the ginseng. In most cases, Rg1/Re < 1 in entire GG and Rg1/Re > 1 in entire MFCG. In addition, the ratio of protopanaxadiol/protopanaxatriol in main root of GG is approximately 1 and, in the main roots of MFCG, the ratio is approximately 2 and, furthermore, Ro/Rb1 of MFCG is lower than that of GG. Analysis of oligosaccharides showed that GG mainly contained sucrose and MFCG mainly contained sucrose and maltose, and the ratio of sucrose to maltose was at least more than 4:1 in GG and less than 4:1 in MFCG in most cases, indicating the characteristics of oligosaccharides of MFCG are primarily affected by its growing environment. The results also showed that ginsenoside Re is most probably the biosynthetic precursor of ginsenoside Rg1 (i.e. Re was synthesized first and then transformed to Rg1 in vivo). CONCLUSION: The characteristics of Rg1/Re and higher maltose can be regarded as one of the characteristics of high quality MFCG, and these characteristics are related to a higher age and the cultivation environment of ginseng. The formation mechanism of these characteristics for GG and MFGG is also discussed. As far as we know, the present study is the first to determine the difference of Rg1/Re and oligosaccharides between MFCG and GG and this provides a reference for the quality control criterion of GG and MFCG. © 2020 Society of Chemical Industry.


Subject(s)
Ginsenosides/chemistry , Oligosaccharides/chemistry , Panax/growth & development , Plant Roots/chemistry , Chromatography, High Pressure Liquid , Gardens , Panax/chemistry , Plant Roots/growth & development , Quality Control
6.
Molecules ; 25(6)2020 Mar 11.
Article in English | MEDLINE | ID: mdl-32168948

ABSTRACT

Psidium guajava, a popular food and medicine dual purposes plant cultivated in tropical and subtropical regions, has been widely used as food crop and folk medicine, such as anti-diabetes agent, around the world. Triterpenoids have been considered as the major active ingredients of P. guajava. In the present study, a high-performance liquid chromatography coupled with diode array and evaporative light scattering detectors (HPLC-DAD-ELSD) method was developed for simultaneous determination of nine triterpenoids in P. guajava. Pressurized liquid extraction (PLE) was performed for sample preparation, and the analysis was achieved on a Cosmosil 5C18-MS-II (Nacalai Tesque, Kyoto, Japan) column eluted with gradient 0.1% aqueous formic acid-methanol system. The drift tube temperature of ELSD was set at 40 °C, and nitrogen flow-rate was at 1.6 L/min. All calibration curves for the analytes showed good linear regression (R2 > 0.9992) within test ranges. The established method was validated for intra-day and inter-day precisions (RSDs < 5%) and accuracy (recovery 94.23-106.87%). The validated method was successfully applied to determinate nine triterpenoids in 15 samples from the leave or fruit of P. guajava. In addition, the α-glucosidase inhibition assay showed good α-glucosidase inhibition activity in almost all the determined triterpenoids. The present study suggested that triterpenoids should be the quality control markers for P. guajava and HPLC-DAD-ELSD was an effective tool for the quality control of P. guajava.


Subject(s)
Drugs, Chinese Herbal/chemistry , Glycoside Hydrolase Inhibitors/chemistry , Hypoglycemic Agents/chemistry , Psidium/chemistry , Triterpenes/chemistry , alpha-Glucosidases/chemistry , Calibration , Chromatography, High Pressure Liquid/instrumentation , Chromatography, High Pressure Liquid/methods , Formates/chemistry , Fruit/chemistry , Glycoside Hydrolase Inhibitors/isolation & purification , Hypoglycemic Agents/isolation & purification , Liquid-Liquid Extraction/methods , Methanol/chemistry , Observer Variation , Plant Leaves/chemistry , Quality Control , Solvents/chemistry , Triterpenes/isolation & purification
7.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-845981

ABSTRACT

Objective: To optimize the infiltration process of Astragalus (Astragalus membranaceus var. mongholicus) medicinal materials by Box-Behnken response surface method. Methods: Based on the HPLC-DAD-ELSD and response surface design method, the qualified rate of decoction pieces, the content of index components and bending inspection were used as comprehensive inspection indicators, and the three factors of infiltration were selected for response surface experimental design to optimize the infiltration process of Astragalus medicinal materials parameter. Results: The best infiltration process was as following: infiltration temperature was 20 ℃, with water addition of 1:0.988 for 6 h. Under this process, the qualified rate of Astragalus pieces was 95.81%, the content of calycosin-7-glucoside was 0.072%, and the content of astragaloside IV was 0.276 %. Combining fingerprint analysis and heat map analysis, the material basis of A. membranaceus var. mongholicus changed during the infiltration process. The infiltration parameters should be strictly controlled during the infiltration process to ensure uniform quality of the pieces. Conclusion: The optimized Astragalus medicinal material infiltration process is stable and feasible with good reproducibility, which can provide a reference for the mass production process development of Astragalus medicinal slices.

8.
China Pharmacy ; (12): 2841-2846, 2020.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-837536

ABSTRACT

OBJECTIVE:To establish a method for simultaneous determination of calycosin glucoside ,ononin,calycosin, formononetin,astragaloside Ⅳ,isoastragaloside Ⅱ,cycloastragenol and isoastragaloside Ⅰ in Astragalus membranaceus before and after bidirectional solid fermentation with Cordyceps kyushuensis ,and to investigate the effects of fermentation on the contents of above 8 components in A. membranaceus . METHODS :HPLC-DAD-ELSD was adopted. The determination was performed on Agilent 5 TC-C18 column with mobile phase consisted of 0.1% formic acid aqueous solution-acetonitrile (gradient elution )at the flow rate of 1 mL/min. The column temperature was set at 30 ℃. DAD detection wavelength was set at 260 nm,ELSD evaporation tube temperature was 100 ℃,atomizer temperature was 80 ℃,carrier gas flow rate was 1.6 L/min;injection volume was 15 μL. RESULTS:The eight components had a good linear relationship within their respective ranges of concentration (all R2>0.999 0); RSDs of precision ,stability and repeatability tests were all less than 3%(n=3 or n=6);the recoveries was 97.88%-101.32%, and RSDs were 1.22%-2.39%(n=6). Setting the content of components in unfermented A. membranaceus as 100%,after bidirectional solid fermentation with C. kyushuensis ,the change rates of 8 components were -98.51%,-96.41%,-94.74%, -96.40%,289.20%,20.25%,-75.05%,562.46%,respectively. CONCLUSIONS :After fermentation with C. kyushuensis ,the contents of active components as astragaloside Ⅳ,isoastragaloside Ⅰ and isoastragaloside Ⅱ can be increased significantly in A. membranaceus .

9.
Chinese Pharmaceutical Journal ; (24): 1057-1062, 2018.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-858281

ABSTRACT

OBJECTIVE: To analyze and identify the compositions using HPLC-DAD/ELSD-ESI-TOF/MS for establishing the multi index quantatitive HPLC fingerprint of the Jinming Tablet, in order to providing scientific basis for its quality control. METHODS: The Agilent SB C18 column (4.6 mm×250 mm, 5 μm) was used with a mobile phase of acetonitrile-0.2% acetic acid in gradient elution, the flow rate was 0.8 mL•min-1, the sample voume was 30 μL, the column temperature was maintaine at 25 ℃, the detection wavelength was set at 280 nm. ESI-TOF/MS positive and negative ion mode scanning was used to qualitatively analyze the components in methanol water extract from Jinming Tablet. RESULTS: Twenty compounds in Jinming Tablet extract could be primarily identified by HPLC-DAD on-line detection, in which five compounds were determined; based on the analysis of multiple batches of samples, the multi index chromatographic fingerprint was established, meanwhile combined with similarity analysis to achieve the quality evaluation of Jinming Tablet. CONCLUSION: The HPLC-DAD/ELSD fingerprint film analysis method for Jinming Tablet is established, which could provide reference for the quality control of the material basis of other compound.

10.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-852364

ABSTRACT

Objective In this paper, HPLC-DAD-ELSD technique was used to establish the chromatography fingerprint of Ilex kudingcha. Methods Shimadzu C18 column (250 mm × 4.6 mm, 5 μm) was used. Acetonitrile-water as the mobile phase; The flow speed was 1.0 mL/min. The detection wavelength was 210 nm and the column temperature was 35 ℃. Results The chromatography fingerprint of Ilex kudingcha from 10 different origins was established. In the chromatography fingerprint with HPLC-DAD of Ilex kudingcha, 18 common peaks were damarcated and the similarities of Ilex kudingcha were between 0.911-0.970, and the chromatography fingerprint with HPLC-ELSD of Ilex kudingcha, 11 common peaks were damarcated and the similarities of Ilex kudingcha were between 0.914-0.962. Chlorogenic acid, kaempferol-3-O-β-D-rhamnoside, isorhamnetin-3-O-β- D-rhamnoside, kudinoside C, kudinoside A, kudinoside E, kudinoside D were confired by LC-MS and binding control. Conclusion The method of precision, reproducibility, stability is accurate, which can be used as the evaluation of the quality of Ilex kudingcha.

11.
Zhongguo Zhong Yao Za Zhi ; 41(23): 4393-4399, 2016 Dec.
Article in Chinese | MEDLINE | ID: mdl-28933118

ABSTRACT

To study the influence of three different drying methods (including 50 ℃-drying, 80 ℃-drying and -70 ℃-freeze-drying methods) on steroidal saponins and homoisoflavonoids in Ophiopogon japonicus,a HPLC-DAD-ELSD-MSn method was investigated to screen and identify the differential components. Through comparing the HPLC chromatograms with that of fresh O. japonicus, 50 ℃-drying medicine was similar with fresh medicine whereas the other two drying methods had great influence on the components of O. japonicus. In this study, 36 differential components were screened, among which 24 constituents(13 homoisoflavonoids and 11 steroidal saponins) were identified via HPLC-LTQ-Orbitrap MS.As a result, it was revealed that different drying methods had significant influences on the components of steroidal saponins and homoisoflavonoids. Among them, 50 ℃-drying method was the most suitable drying approach when the stability of components, cost and practicability were considered.


Subject(s)
Desiccation/methods , Flavonoids/analysis , Ophiopogon/chemistry , Saponins/analysis , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal/chemistry , Mass Spectrometry
12.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-272682

ABSTRACT

To study the influence of three different drying methods (including 50 ℃-drying, 80 ℃-drying and -70 ℃-freeze-drying methods) on steroidal saponins and homoisoflavonoids in Ophiopogon japonicus,a HPLC-DAD-ELSD-MSn method was investigated to screen and identify the differential components. Through comparing the HPLC chromatograms with that of fresh O. japonicus, 50 ℃-drying medicine was similar with fresh medicine whereas the other two drying methods had great influence on the components of O. japonicus. In this study, 36 differential components were screened, among which 24 constituents(13 homoisoflavonoids and 11 steroidal saponins) were identified via HPLC-LTQ-Orbitrap MS.As a result, it was revealed that different drying methods had significant influences on the components of steroidal saponins and homoisoflavonoids. Among them, 50 ℃-drying method was the most suitable drying approach when the stability of components, cost and practicability were considered.

13.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-854139

ABSTRACT

Objective: To establish the chromatography fingerprint of Polygoni Cuspidati Rhizoma et Radix with hyphenated technique of HPLC-DAD-ELSD and to evaluate Polygoni Cuspidati Rhizoma et Radix from 10 different origins. Methods: Luna C18 (2) column (250 mm × 4.6 mm, 5 μm) was used. Mobile phase was acetonitrile-H2O; Flow speed was 1.0 mL/min; Temperature of column was set at 35℃; Detective wavelength was at 254 nm; Injection volume was 10 μL. The temperature of drift tube was 109℃ and the flow speed was 3.0 L/min. Results: The chromatography fingerprint of Polygoni Cuspidati Rhizoma et Radix from 10 different origins was established. In the chromatography fingerprint with HPLC-DAD of Polygoni Cuspidati Rhizoma et Radix, 19 common peaks were demarcated and the similarities of Polygoni Cuspidati Rhizoma et Radix were between 0.938-0.993. In the chromatography fingerprint with HPLC-ELSD of Polygoni Cuspidati Rhizoma et Radix, 14 common peaks were demarcated and the similarities of Polygoni Cuspidati Rhizoma et Radix were between 0.905-0.999. Polydatin, resveratrol, emodin-8-O-β-D-glucoside, physcion-8-O-β-D-glucoside, emodin, and physcion were identified. Conclusion: The method is accurate and stable, which can be used as the evidence for the quality evaluation of Polygoni Cuspidati Rhizoma et Radix.

14.
China Pharmacist ; (12): 867-869, 2015.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-669786

ABSTRACT

Objective:To establish an HPLC-DAD-ELSD method for the simultaneous determination of neomycin sulfate and hy-drochloric dyclonine in compound Twaln ointments. Methods:The assay was performed on an Agilent ZOR BAXSB-C18 column(250 mm × 4. 6 mm, 5μm) with acetonitrile-water as the mobile phase with gradient elution at a flow rate of 1. 0 ml·min-1 . The detection wavelength of DAD was 282 nm. The evaporator temperature of ELSD was set at 50℃ and the nebulizer temperature was set at 60℃with the gas flow rate of 1. 6 L·min-1 . The column temperature was kept at 35℃. Results:The linear range of neomycin sulfate was 141. 54-323. 52 μg·mL-1(r=0. 999 6) with the average recovery of 98. 87%(RSD=0. 95%, n=9). The linear range of hydro-chloric dyclonine was 28. 00-64. 00 μg·mL-1(r=0. 999 6) with the average recovery of 99. 57%(RSD=1. 10%, n=9). Conclu-sion:The method is accurate, sensitive and reproducible, and under the same chromatographic conditions, the determination of all the active ingredients in compound Twaln ointments is achieved, which provides basis for the quality control.

15.
Chin J Nat Med ; 12(7): 525-34, 2014 Jul.
Article in English | MEDLINE | ID: mdl-25053552

ABSTRACT

AIM: To develop and validate a high performance liquid chromatography (HPLC) coupled with diode array and evaporative light scattering detectors (DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes (namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair (ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column (4.6 mm × 250 mm, 5 µm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min(-1) at 260 nm. The drift tube temperature of ELSD was set to 60 °C and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds (phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.


Subject(s)
Alkaloids/analysis , Chromatography, High Pressure Liquid/methods , Drugs, Chinese Herbal/analysis , Glycosides/analysis , Xanthones/analysis , Chromatography, High Pressure Liquid/instrumentation
16.
China Pharmacist ; (12): 782-785, 2014.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-445993

ABSTRACT

Objective:To develop an HPLC-DAD-ELSD method for the determination of nitidine chloride, 5-ethoxychelerythrine, bergeninum and ardisiacrispin A in Shangtong tinctures ( STD) . Methods: A Hypersil C18 column was used as the chromatographic column, the flow rate was 0. 8 ml·min-1 . For nitidine chloride and 5-ethoxychelerythrine, the mobile phase A consisted of acetoni-trile,the mobile phase B consisted of 0. 1% formic acid-triethylamine (pH 4. 5),and the DAD detection wavelength was at 273 nm. For bergeninum and ardisiacrispin A, the mobile phase consisted of methanol-water(25∶75), the temperature of drift tube was set at 95℃, and the gas flow (N2) was set at 2. 5 SLPM·min-1. Results:There was a good linear relationship between the concentration and peak area for nitidine chloride and 5-ethoxychelerythrine within the range of 0. 021-0. 426 μg (r=0. 999 5) and 0. 075-1. 494 μg (r=0. 999 8), respectively. The average recovery was 99. 22%(RSD=0. 64%) and 98. 61%(RSD=0. 46%), respectively. There was a good linear relationship between the concentration and peak area for bergeninum and ardisiacrispin A within the range of 0. 215-4. 304 μg(r=0. 999 3) and 0. 286-5. 728 μg(r=0. 999 7), respectively. The average recovery was 99. 15%(RSD=0. 77%) and 99. 25%(RSD=0. 56%) accordingly. Conclusion:The method is accurate, sensitive and reproducible, and can be used in the de-termination of nitidine chloride, 5-ethoxychelerythrine, bergeninum and ardisiacrispin A in STD.

17.
Article in English | WPRIM (Western Pacific) | ID: wpr-812237

ABSTRACT

AIM@#To develop and validate a high performance liquid chromatography (HPLC) coupled with diode array and evaporative light scattering detectors (DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes (namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair (ZB).@*METHOD@#Chromatographic separation was performed on a Diamonsil C18 column (4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min(-1) at 260 nm. The drift tube temperature of ELSD was set to 60 °C and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy.@*RESULTS@#The HPLC-DAD-ELSD method allowed the quantification of ten compounds (phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples.@*CONCLUSION@#This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.


Subject(s)
Alkaloids , Chromatography, High Pressure Liquid , Methods , Drugs, Chinese Herbal , Glycosides , Xanthones
18.
Article in Chinese | WPRIM (Western Pacific) | ID: wpr-579548

ABSTRACT

Objective To establish the HPLC-DAD-ELSD fingerprint of Radix astragali,provide new methods for science quality control of the medicinal materials.Methods Application of HPLC-DAD-ELSD techniques were connected in series.The mobile phase A: 10% acetonitrile,B: 90% acetonitrile,detecting wavelength: 265 nm,flow rate: 1 mL/min,column temperature: 35 ℃,sample size: 20 ?L,gain: 20,tube: 55 ℃,neb: 65%,air pressure: 2.068 5?105 Pa.The mutual mode was established depending on ten Astragalus samples from different growing areas in Gansu.The software "Similarity Evaluation System for Chromatographic Fingerfrint of Chinese Materia Medica" was applied to analyzing.ResultsThe established method is good for the separation of saponins,flavonoids from Radix Astragali,and simultaneous determination of the two different components in one sample injection.The similarity of different batches of medicinal materials is fit for the requirement.Conclusion The method is workable to simultaneously determine saponins and flavonoids fingerprint from Radix Astragali,and to control its quality.

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