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1.
Molecules ; 29(5)2024 Feb 29.
Artículo en Inglés | MEDLINE | ID: mdl-38474586

RESUMEN

Cyclic adenosine monophosphate (cAMP) is an important second messenger in cells, mediating various stimulation signals such as the growth and development of organisms and stress and participating in regulating various biological processes of cells. This article explores the quantitative determination of cAMP in plants using High-Performance Liquid Chromatography (HPLC) and applies this method to analyzing the changes in cAMP content during the process of plant response to the bacterial quorum sensing signal N-acyl homoserine lactone (AHL). Research has shown that the optimal detection conditions for HPLC are as follows: the chromatographic column is Venusil MP C18 (2), the mobile phase is methanol-water (0.1% trifluoroacetic acid) (v:v, 10:90), the detection wavelength is 259 nm, the column temperature is 35 °C, and the flow rate is 0.8 mL/min. The precision of the standard sample of this method is 98.21%, the precision of the sample is 98.87%, and the recovery rate is 101.067%. The optimal extraction conditions for cAMP in Arabidopsis are to use 15% methanol ultrasonic extraction for 10 min, followed by a 40 °C water bath for 4 h. Bacterial AHL signal processing can significantly stimulate an increase in cAMP levels in Arabidopsis leaves and roots. The establishment of HPLC detection methods for the cAMP content in plants is of great significance for in-depth research on the signal transduction mechanisms of plant-bacterial interactions.


Asunto(s)
Acil-Butirolactonas , Arabidopsis , Cromatografía Líquida de Alta Presión , Metanol , Bacterias , Plantas , AMP Cíclico , Agua , Adenosina Monofosfato
2.
Zhongguo Zhong Yao Za Zhi ; 48(9): 2471-2479, 2023 May.
Artículo en Chino | MEDLINE | ID: mdl-37282876

RESUMEN

In order to comprehensively evaluate the quality of Viticis Fructus, this study established HPLC fingerprints and evaluated the quality of 24 batches of Viticis Fructus samples from different species by similarity evaluation and multivariate statistical analysis(PCA, HCA, PLS-DA). On this basis, an HPLC method was established to compare the content differences of the main components, including casticin, agnuside, homoorientin, and p-hydroxybenzoic acid. The analysis was performed on the chromatographic column(Waters Symmetry C_(18)) with a gradient mobile phase of acetonitrile(A)-0.05% phosphoric acid solution(B) at the flow rate of 1 mL·min~(-1) and detection wavelength of 258 nm. The column temperature was 30 ℃ and the injection volume was 10 µL. The HPLC fingerprint of 24 batches of Viticis Fructus samples was established with 21 common peaks, and nine peaks were identified. Similarity analysis was carried out based on chromatographic data of 24 batches of chromatographic data of Viticis Fructus, and the results showed that except for DYMJ-16, the similarity of Vitex trifolia var. simplicifolia was ≥0.900, while that of V. trifolia was ≤0.864. In addition, the similarity analysis of two different species showed that the similarity of 16 batches of V. trifolia var. simplicifolia was 0.894-0.997 and that of the eight batches of V. trifolia was between 0.990 and 0.997. The results showed that the similarity of fingerprints of these two species was different, but the similarity between the same species was good. The results of the three multivariate statistical analyses were consistent, which could distinguish the two different species. The VIP analysis results of PLS-DA showed that casticin and agnuside contributed the most to the distinction. The content determination results showed that there was no significant difference in the content of homoorientin and p-hydroxybenzoic acid in Viticis Fructus from different species, but the content of casticin and agnuside was significantly different in different species(P<0.01). The content of casticin was higher in V. trifolia var. simplicifolia, while agnuside was higher in V. trifolia. The findings of this study show that there are differences in fingerprint similarity and component content of Viticis Fructus from different species, which can provide references for the in-depth study of the quality and clinical application of Viticis Fructus.


Asunto(s)
Medicamentos Herbarios Chinos , Vitex , Medicamentos Herbarios Chinos/química , Cromatografía Líquida de Alta Presión/métodos , Frutas/química , Vitex/química
3.
Zhongguo Zhong Yao Za Zhi ; 48(8): 2116-2125, 2023 Apr.
Artículo en Chino | MEDLINE | ID: mdl-37282900

RESUMEN

This study aims to separate and characterize self-assembled nanoparticles(SAN) from Shaoyao Gancao Decoction(SGD) and determine the content of active compounds. Further, we aimed to observe the therapeutic effect of SGD-SAN on imiquimod-induced psoriasis in mice. The separation of SGD was performed by dialysis, and the separation process was optimized by single factor experiment. The SGD-SAN isolated under the optimal process was characterized, and the content of gallic acid, albiflorin, paeoniflorin, liquiritin, isoliquiritin apioside, isoliquiritin, and glycyrrhizic acid in each part of SGD was determined by HPLC. In the animal experiment, mice were assigned into a normal group, a model group, a methotrexate group(0.001 g·kg~(-1)), and SGD, SGD sediment, SGD dialysate, and SGD-SAN groups of different doses(1, 2, and 4 g·kg~(-1)) respectively. The psoriasis grade of mice was evaluated based on the pathological changes of skin lesions, the content of inflammatory cytokines, organ index and other indicators. The results showed that SAN obtained by centrifugation at 13 000 r·min~(-1) for 30 min was stable after dialysis for 4 times, which were uniform spherical nanoparticles with the particle size of(164.43±1.34) nm, the polydispersity index of(0.28±0.05), and the Zeta potential of(-12.35±0.80) mV. The active compound content accounted for more than 70% of SGD. Compared with the model group, SAN and SGD decreased the skin lesion score, spleen index, and inflammatory cytokine levels(P<0.05 or P<0.01) and alleviated the skin thickening and infiltration of inflammatory cells. However, the sediment group and the dialysate group had no obvious effect. SGD showed a good therapeutic effect on imiquimod-induced psoriasis in mice, and SAN demonstrated the effect equivalent to SGD in a dose-dependent manner. Therefore, we conclude that the SAN formed during decocting is the main active form of SGD, which can lower the levels of inflammatory cytokines, promote the normal differentiation of keratinocytes, and reduce the infiltration of inflammatory cells in the treatment of psoriasis lesions in mice.


Asunto(s)
Medicamentos Herbarios Chinos , Ratones , Animales , Imiquimod , Medicamentos Herbarios Chinos/farmacología , Ácido Glicirrínico , Cromatografía Líquida de Alta Presión/métodos
4.
Heliyon ; 9(3): e14156, 2023 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-36925510

RESUMEN

To establish the freeze-drying process and the HPLC method to determine the main effective components and content of freeze-dried Polygonatum sibiricum of China. The results show that the freeze-drying process is a slice thickness at 3 mm, boiling time 2 min, pre-freezing temperature at -35 °C, low-temperature holding at -10 °C, low temperature sublimation at 10 °C and drying temperature at 35 °C. The optimum HPLC conditions of freeze-dried Polygonatum sibiricum was SepaxGp-C18 (4.6 × 250 mm, 5 µm), gradient elution of mobile phase A (acetonitrile)-B (ultra-pure water), detection wavelength of 254 nm, the flow rate of 1 mL/min, column temperature of at 30 °C and injection volume of 10 µL. Polygonatum sibiricum from different producing areas contains a variety of amino acids, diosgenin, sugars, and other active ingredients. The protein content of Polygonatum sibiricum from Yunnan Pu'er is the highest among them, and that of Shangluo in Shaanxi is the lowest. The total sugar content of Polygonatum sibiricum in Puer is the highest, while that of Polygonatum sibiricum in Wenshan is the lowest. And the diosgenin of Polygonatum sibiricum in Lijiang is the highest. In this study, the freeze-drying process of Polygonatum sibiricum was established, and the main effective components and contents of freeze-dried Polygonatum sibiricum was determined as the better HPLC method, provided theoretical and technical support for the rational development and utilization of Polygonatum sibiricum.

5.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-981323

RESUMEN

In order to comprehensively evaluate the quality of Viticis Fructus, this study established HPLC fingerprints and evaluated the quality of 24 batches of Viticis Fructus samples from different species by similarity evaluation and multivariate statistical analysis(PCA, HCA, PLS-DA). On this basis, an HPLC method was established to compare the content differences of the main components, including casticin, agnuside, homoorientin, and p-hydroxybenzoic acid. The analysis was performed on the chromatographic column(Waters Symmetry C_(18)) with a gradient mobile phase of acetonitrile(A)-0.05% phosphoric acid solution(B) at the flow rate of 1 mL·min~(-1) and detection wavelength of 258 nm. The column temperature was 30 ℃ and the injection volume was 10 μL. The HPLC fingerprint of 24 batches of Viticis Fructus samples was established with 21 common peaks, and nine peaks were identified. Similarity analysis was carried out based on chromatographic data of 24 batches of chromatographic data of Viticis Fructus, and the results showed that except for DYMJ-16, the similarity of Vitex trifolia var. simplicifolia was ≥0.900, while that of V. trifolia was ≤0.864. In addition, the similarity analysis of two different species showed that the similarity of 16 batches of V. trifolia var. simplicifolia was 0.894-0.997 and that of the eight batches of V. trifolia was between 0.990 and 0.997. The results showed that the similarity of fingerprints of these two species was different, but the similarity between the same species was good. The results of the three multivariate statistical analyses were consistent, which could distinguish the two different species. The VIP analysis results of PLS-DA showed that casticin and agnuside contributed the most to the distinction. The content determination results showed that there was no significant difference in the content of homoorientin and p-hydroxybenzoic acid in Viticis Fructus from different species, but the content of casticin and agnuside was significantly different in different species(P<0.01). The content of casticin was higher in V. trifolia var. simplicifolia, while agnuside was higher in V. trifolia. The findings of this study show that there are differences in fingerprint similarity and component content of Viticis Fructus from different species, which can provide references for the in-depth study of the quality and clinical application of Viticis Fructus.


Asunto(s)
Medicamentos Herbarios Chinos/química , Cromatografía Líquida de Alta Presión/métodos , Frutas/química , Vitex/química
6.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-981343

RESUMEN

This study aims to separate and characterize self-assembled nanoparticles(SAN) from Shaoyao Gancao Decoction(SGD) and determine the content of active compounds. Further, we aimed to observe the therapeutic effect of SGD-SAN on imiquimod-induced psoriasis in mice. The separation of SGD was performed by dialysis, and the separation process was optimized by single factor experiment. The SGD-SAN isolated under the optimal process was characterized, and the content of gallic acid, albiflorin, paeoniflorin, liquiritin, isoliquiritin apioside, isoliquiritin, and glycyrrhizic acid in each part of SGD was determined by HPLC. In the animal experiment, mice were assigned into a normal group, a model group, a methotrexate group(0.001 g·kg~(-1)), and SGD, SGD sediment, SGD dialysate, and SGD-SAN groups of different doses(1, 2, and 4 g·kg~(-1)) respectively. The psoriasis grade of mice was evaluated based on the pathological changes of skin lesions, the content of inflammatory cytokines, organ index and other indicators. The results showed that SAN obtained by centrifugation at 13 000 r·min~(-1) for 30 min was stable after dialysis for 4 times, which were uniform spherical nanoparticles with the particle size of(164.43±1.34) nm, the polydispersity index of(0.28±0.05), and the Zeta potential of(-12.35±0.80) mV. The active compound content accounted for more than 70% of SGD. Compared with the model group, SAN and SGD decreased the skin lesion score, spleen index, and inflammatory cytokine levels(P<0.05 or P<0.01) and alleviated the skin thickening and infiltration of inflammatory cells. However, the sediment group and the dialysate group had no obvious effect. SGD showed a good therapeutic effect on imiquimod-induced psoriasis in mice, and SAN demonstrated the effect equivalent to SGD in a dose-dependent manner. Therefore, we conclude that the SAN formed during decocting is the main active form of SGD, which can lower the levels of inflammatory cytokines, promote the normal differentiation of keratinocytes, and reduce the infiltration of inflammatory cells in the treatment of psoriasis lesions in mice.


Asunto(s)
Ratones , Animales , Imiquimod , Medicamentos Herbarios Chinos/farmacología , Ácido Glicirrínico , Cromatografía Líquida de Alta Presión/métodos
7.
Ceska Slov Farm ; 70(3): 85-92, 2021.
Artículo en Inglés | MEDLINE | ID: mdl-34418945

RESUMEN

The paper draws attention to the correlations between the results of instrumental colour measurements and the content of some biologically active organic substances (carotenoids, chlorophyll, anthocyanins, curcuminoids, etc.) in natural products and products of natural origin. After supplementation by regression analysis and calibration, sufficiently close correlations can lead to the development of procedures for rapid determination of the content of these substances and their groups by colour measurement without more demanding sample treatment.


Asunto(s)
Productos Biológicos , Antocianinas , Color
8.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-906764

RESUMEN

@#A deuterated internal standard quantitative analysis method based on liquid-liquid extraction-ultra performance liquid chromatography-tandem mass spectrometry (LLE-UPLC-MS/MS) for simultaneous determination of 10 illicit drugs in wastewater was established.Wastewater samples were concentrated by liquid-liquid extraction with dichloromethane: ethyl acetate (1∶1), and separated by a linear gradient of 0.1% formic acid-5 mmol/L ammonium formate aqueous solution and acetonitrile on a C18 column. The samples were then detected by ESI positive ion mode and multiple reaction monitoring mode (MRM) for quantitative analysis.All analytes had a good linear relationship (r ≥ 0.995 7) within the range of their respective standard curves; the limit of quantification was 1 ng/L (except amphetamine at 2.5 ng/L); the relative recovery rate ranged from 96.36% to 106.43%, and the intra- and inter-day precisions were less than 4.70%.This method is accurate, reliable and reproducible, and is suitable for the quantitative determination of 10 illicit drugs in wastewater.It is also suitable for wastewater with complex matrixes that affect solid phase extraction and enrichment.It provides a new analytical method for real-time monitoring of drug abuse.

9.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-906765

RESUMEN

@#TA method for the content determination of methionine sulfoxide and methionine sulfone in compound amino acid injection (18AA-II) was established in order to investigate their level in 155 batches of this product, and to explore the reason for the generation of these two impurities.The determination was performed on an Agilent Poroshell 120 EC-C18 column with mobile phases of sodium acetate/tetrahydrofuran solution (A) and sodium acetate solution -acetonitrile-methanol (B, 200∶400∶400) (gradient elution) at the flow rate of 0.5 mL/min.The excitation wavelength and the emission wavelength of the fluorescence detector were 233 nm and 441 nm, respectively.The column temperature was 40 °C, and the injection volume was 8 μL.The contents of methionine sulfoxide and methionine sulfone from 155 batches of compound amino acid injection (18AA-II) was determined using this method, and the residual oxygen content was detected by headspace gas analyzer.The results showed that the linear range of methionine sulfoxide and methionine sulfone were 0.128 1-10.250 0 μg/mL (r = 0.999 9) and 0.261 0-10.440 0 μg/mL (r = 0.999 8), respectively.The limits of quantitation were 0.13 μg/mL and 0.26 μg/mL, respectively; the limits of detection were 0.04 μg/mL and 0.09 μg/mL, respectively.RSDs of precision, stability and repetitive test were all lower than 1.3%.The recoveries ranged 98.00%-100.79% (RSD = 1.15%, n = 9) and 98.19%-102.31% (RSD = 1.33%, n = 9).The content level of oxidized related substances from different manufacturers showed significant difference, showing relevance with the residual oxygen content to some extent, yet no significant correlation with the added amount of antioxygen (sodium pyrosulfite).The method is validated to be useful for the content control of methionine sulfoxide and methionine sulfone in compound amino acid injection (18AA-II).It is quite necessary to include the determination of oxidized related substance into the quality specification.Manufacturers should strengthen the control of remaining oxygen in their products.

10.
J Pharm Biomed Anal ; 193: 113636, 2021 Jan 30.
Artículo en Inglés | MEDLINE | ID: mdl-33221574

RESUMEN

The screening of marker compound is of great significance to the quality control of traditional Chinese medicine (TCM). One approach which combines fingerprint and biological evaluation has developed rapidly. Multi-wavelength fusion fingerprints and antioxidant activity screening are integrated in this study to evaluate the quality of NAODESHENG. Characteristic multiwavelength fusion fingerprints of 14 batches of samples were generated at five different wavelengths and evaluated by quantitative fingerprinting with ultra-performance liquid chromatography (UPLC). In the quantitative fingerprinting method, 21 components in NAODESHENG were qualitatively and quantitatively analyzed by external standard method. The antioxidant activities of these 21 components was determined by pre-column antioxidant activity test. Multivariate statistical methods such as hierarchical clustering analysis and principal component analysis(PCA) was used to reduce the dimensions and variables from a large number of original data to screening marker compound with bioactivity. Based on the above results, it is suggested that 3'-Methoxy Puerarin and 11 other components should be used as the quality marker of NAODESHENG. This study demonstrates the feasibility of multi-wavelength fusion fingerprinting combined with antioxidant activity analysis, which associates quality control with bioactivity, providing a reliable and efficient method for quantitative assessment of TCM quality consistency.


Asunto(s)
Antioxidantes , Medicamentos Herbarios Chinos , Cromatografía Líquida de Alta Presión , Cromatografía Liquida
11.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-821078

RESUMEN

@#A reversed phase HPLC method for determination of hydroxylsafflower yellow A in safflower W/O cream was established. The column was Zorbax Eclipse C18 column(4. 6 mm×250 mm, 5 μm), and the mobile phase was composed of methanol, acetonitrile and 0. 02% phosphoric acid solution(26 ∶2〓 ∶72). The flow rate of mobile phase was set at 1. 0 mL/min, and the column temperature was kept at 55 °C. The detection wavelength was 403 nm. Safflower W/O cream was successively demulsified with methanol at high temperature and followed by the addition of purified water for the extraction. The results showed that the excipients did not interfere with the chromatographic peak of hydroxylsafflower yellow A. Hydroxylsafflower yellow A presented a good linear relationship in the range of 1. 236- 12. 36 μg/mL(y=156. 17x+1. 198 3, r=0. 999 5), and the detection limit was 23. 6 ng/mL with the quantitative limit of 118 ng/mL. The percentage of extracting recovery was in the range of 99. 7% to 103. 3%. The precision RSD was 0. 12%(n=6), and the sample stability was acceptable when being stored at room temperature for 24 h. The developed method in this study was simple, rapid, accurate and reproducible, and can be used for the determination of hydroxylsafflower yellow A in safflower W/O cream.

12.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-825141

RESUMEN

@#An analytical liquid-liquid extraction-gas chromatography–mass spectrometry (LLE-GC-MS) method was established for the determination of genotoxic impurities including methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IMS) in methanesulfonic acid. An Agilent HP-1MS capillary column (30 m × 0.32 m, 1 μm) was used for separating the analytes by programmed heating with the inlet temperature of 220 °C. Mass spectrometry was operated in positive ion mode, and selective ion monitors were set at m/z 80 for MMS, m/z 79 for EMS, m/z 123 for IMS and m/z 56 for internal standard butyl methanesulfonate (BMS). Results showed that the baseline separation of MMS, EMS and IMS was achieved, and the blank extraction solution had no interference; good linearity was achieved in the range of 37-1 480 ng/mL for three alkyl methanesulfonates; The mean recoveries of MMS, EMS, IMS were 104.99%, 107.26%,108.85%, respectively, with RSD ≤ 4.54%. The established method has the characteristics of specific, sensitive, accurate, stable and good versatility, and has been used for the detection and control of alkyl methanesulfonate impurities in methanesulfonic acid from a variety of manufacturers.

13.
Ceska Slov Farm ; 68(4): 157-160, 2019.
Artículo en Inglés | MEDLINE | ID: mdl-31822108

RESUMEN

In the European Pharmacopoeia (Ph. Eur.) there is no prescribed number of parallel determinations of the content of active substances and excipients. The authors suggest adding at least three determinations. The results of parallel determinations suggest to test for outliers before using test based on the ratio of the range of results (p = 0.95) and not to compare individual results with the tolerance limits given in Ph. Eur., but with their arithmetic mean. Furthermore, they propose to extend the Chapter 5.3. of the European Pharmacopoeia so as to be applicable not only to bioassays, but also to chemical, physicochemical and physical assays and tests, starting with the content of active substances and excipients.


Asunto(s)
Excipientes/normas , Preparaciones Farmacéuticas/normas , Europa (Continente) , Farmacopeas como Asunto
14.
Zhongguo Zhong Yao Za Zhi ; 43(13): 2740-2746, 2018 Jul.
Artículo en Chino | MEDLINE | ID: mdl-30111025

RESUMEN

An HPLC method was developed for the determination of iridoid glycosides (loganin acid, loganin, sweroside) and saponins (asperosaponin Ⅵ) in the wild Dipsacus asper. A total of 108 samples consecutive growing 12 month were collected in 9 plots in Wulong district of Chongqing. Subsequent analysis of the content of loganin acid, loganin, sweroside and asperosaponin Ⅵ was performed by HPLC to evaluate the quality. In addition, 20 climate data provided by the world climate database (http://www.worldclim.org/) was analyzed to deduce the correlation between the growing environment factors and the active ingredient content accumulation of D. asperoides and choose the apposite growing environment for D. asper. The range of active ingredient content in wild D. asper were 0.01%-3.80%(loganin acid), 0.08%-0.62%(loganin), 0.12%-0.78%(sweroside), 0.64%-5.26%(asperosaponin Ⅵ). The highest content of these active ingredients was concentrated from February to April, with 2.64% of loganin acid, 0.36% of loganin), 0.57% of sweroside, and 3.09% of asperosaponin Ⅵ. The method used for determination of the active ingredient content in D. asper was simple and convenient with accurate result. The selection of the quadrats is scientific and reasonable and can be used for the analysis of the contents of the wild D. asper, thus provide a reference for quality evaluation of D. asper and protection of D. asper resources.


Asunto(s)
Dipsacaceae , Medicamentos Herbarios Chinos , Cromatografía Líquida de Alta Presión , Ecosistema
15.
Zhongguo Zhong Yao Za Zhi ; 43(9): 1769-1773, 2018 May.
Artículo en Chino | MEDLINE | ID: mdl-29902884

RESUMEN

This study aimed to develop an HPLC method for simultaneous determination of the 3 components in Ziziphora bungeana. The optimum HPLC condition was as follows:ZORBAX SB-C18 column(4.6 mm×250 mm, 5.0 µm)with gradient elution of methanol (A)-0.2% glacial acetic acid (B), detection wavelength 340 nm,column temperature 30 °C, flow rate 1 mL·min⁻¹. There were good linearity between peak areas and injection quantity of caffeic acid, rosmarinic acid, and linarin in the range of 2-40 mg·L⁻¹ï¼ˆr=0.999 9), 3-60 mg·L⁻¹ï¼ˆr=1), 7-140 mg·L⁻¹ï¼ˆr=0.999 9), respectively. The average recoveries were 100.9%(RSD 1.3%),98.25%(RSD 2.0%),and 98.73%(RSD 1.5%), respectively. The HPLC method was stable and accurate, which could be used to detect caffeic acid,rosmarinic acid, and linarin in Ziziphora bungeana.


Asunto(s)
Medicamentos Herbarios Chinos , Lamiaceae , Cromatografía Líquida de Alta Presión
16.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-687391

RESUMEN

An HPLC method was developed for the determination of iridoid glycosides (loganin acid, loganin, sweroside) and saponins (asperosaponin Ⅵ) in the wild Dipsacus asper. A total of 108 samples consecutive growing 12 month were collected in 9 plots in Wulong district of Chongqing. Subsequent analysis of the content of loganin acid, loganin, sweroside and asperosaponin Ⅵ was performed by HPLC to evaluate the quality. In addition, 20 climate data provided by the world climate database (http://www.worldclim.org/) was analyzed to deduce the correlation between the growing environment factors and the active ingredient content accumulation of D. asperoides and choose the apposite growing environment for D. asper. The range of active ingredient content in wild D. asper were 0.01%-3.80%(loganin acid), 0.08%-0.62%(loganin), 0.12%-0.78%(sweroside), 0.64%-5.26%(asperosaponin Ⅵ). The highest content of these active ingredients was concentrated from February to April, with 2.64% of loganin acid, 0.36% of loganin), 0.57% of sweroside, and 3.09% of asperosaponin Ⅵ. The method used for determination of the active ingredient content in D. asper was simple and convenient with accurate result. The selection of the quadrats is scientific and reasonable and can be used for the analysis of the contents of the wild D. asper, thus provide a reference for quality evaluation of D. asper and protection of D. asper resources.

17.
China Pharmacy ; (12): 1213-1217, 2018.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-704767

RESUMEN

OBJECTIVE:To establish the method for simultaneous determination of 9 components in Huichun yuzi granules. METHODS:LC-MS/MS method was adopted. The determination was performed on Shim-pack XR-ODS C18column with column temperature of 30 ℃. The sample size was 5 μL,and ion source as electrospray ion source;MRM mode was adopted. The acetonitrile-water was used as mobile phase for ferulic acid,rutin,paeonol,icariin and schisandrin(gradient elution);positive ion mode monitoring was conducted. The methanol-0.1% fomic acid water was used as mobile phase for naringin,verbascoside, amygdalin and protocatechuic acid(gradient elution);negative ion mode monitoring was conducted. RESULTS:The linear ranges of ferulic acid,rutin,paeonol,icariin,schisandrin,naringin,verbascoside,amygdalin and protocatechuic acid were 0.499 5-500, 25-1 000,0.245 9-250,5.185 1-1 000,0.981 9-1 000,0.248 1-125,2.510 4-250,10-2 500,4.999 7-1 000 ng/mL(r≥0.997 8), respectively. The limits of detection were 0.075,0.30,0.072,0.015,0.015,0.075,0.15,0.30,0.15 ng/mL,respectively;the limits of quantitation were 0.25,1.00,0.24,0.51,0.49,0.25,0.50,0.99,0.49 ng/mL,respectively. The recoveries rate were 91.39%-103.56%(RSD=1.03%-3.67%,n=6).RSDs of stability test ranged 1.4%-3.4%(n=6)within 48 h at room temperature. CONCLUSIONS:The method is rapid,sensitive and reproducible,and can be used for content determination of 9 components in Huichun yuzi granules.It can be used for quality control of Huichun yuzi granules.

18.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-690715

RESUMEN

This study aimed to develop an HPLC method for simultaneous determination of the 3 components in Ziziphora bungeana. The optimum HPLC condition was as follows:ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5.0 μm)with gradient elution of methanol (A)-0.2% glacial acetic acid (B), detection wavelength 340 nm,column temperature 30 °C, flow rate 1 mL·min⁻¹. There were good linearity between peak areas and injection quantity of caffeic acid, rosmarinic acid, and linarin in the range of 2-40 mg·L⁻¹(=0.999 9), 3-60 mg·L⁻¹(=1), 7-140 mg·L⁻¹(r=0.999 9), respectively. The average recoveries were 100.9%(RSD 1.3%),98.25%(RSD 2.0%),and 98.73%(RSD 1.5%), respectively. The HPLC method was stable and accurate, which could be used to detect caffeic acid,rosmarinic acid, and linarin in Ziziphora bungeana.

19.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-811728

RESUMEN

@#To develop a rapid and sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of endogenous glutathione in rat plasma. Glycyltyrosine was used as the internal standard(IS)and 4-(N-maleimido)phenyl trimethylammonium iodide(MPTA)was used as the derivation reagent. Chromatographic separation was achieved on a Zorbax HILIC PLUS column(4. 6 mm×100 mm, 3. 5 μm)and the mobile phase consisted of acetonitrile and 0. 1% formic acid(75 ∶25)pumped at a flow rate of 1. 0 mL/min. Detection was carried out on a triple quadrupole tandem mass spectrometer by selected reaction monitoring(SRM)in the can meet positive ion mode. The linearity ranged from 3. 000 to 2 000 ng/mL(r=0. 997 1); and the limit of detection of glutathione in rat plasma was 10 pmol/L. Matrix effect, stability, precision and accuracy of the method met the requirements. The proposed method was proved to be selective and sensitive, which is suitable for the quantification of endogenous glutathione in rat plasma.

20.
Artículo en Chino | WPRIM (Pacífico Occidental) | ID: wpr-704307

RESUMEN

In order to research the related substances of dabigatran etexilate mesylate,seven related compounds were synthesized and the related detection methods were established (Using XBridge C18 as the column,methanol-0.01mol/L potassium dihydrogen phosphate as the mobile phase Gradient elution,detection wavelength of 310 nm).The solvents and the injection volume were also screened.Results showed that the established method could separate the dabigatran etexilate mesylate and seven compounds completely,and the reproducibility was good and the accuracy was high,which was suitable for the detection of the related substances of dabigatran etexilate mesylate.

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