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1.
J Chromatogr A ; 1218(8): 1131-8, 2011 Feb 25.
Artigo em Inglês | MEDLINE | ID: mdl-21256495

RESUMO

Polyacetylenes are main toxic ingredients in Bupleurum longiradiatum, a poisonous plant that has ever been misused as substitutes for Chaihu (Bupleuri Radix). For the first time, a high-performance liquid chromatography method coupled with diode array detector and mass spectrometry (HPLC-DAD-MS) was developed for qualitative and quantitative analysis of nine polyacetylenes in Bupleurum species. All references, including two new polyacetylenes, were isolated from B. longiradiatum and purified using a semi-preparation HPLC chromatography. The analysis was performed on a TSKgel ODS-100V C18 column (3 µm, 150 mm x 4.6 mm i.d.) using a gradient system of acetonitrile and water, with diode array detection (254 nm). The method was validated for linearity, precision, accuracy, limit of detection and quantification. A total of 27 Bupleurum samples were examined with this method, which showed a great variety in the distribution and contents of the polyacetylenes. It was found that polyacetylenes (1-8) were the main ingredients in B. longiradiatum, while a few kinds of polyacetylenes (5-8) were also identified in B. smithii, B. smithii var. parvifolium, B. bicaule and B. angustissimum. However, no polyacetylenes (1-9) were detected in the authentic Chaihu samples and the other Bupleurum species. The results indicated that the toxic B. longiradiatum could readily be distinguished from other medicinal Bupleurum species based on the polyacetylene profiles, and the guidelines and quality control of polyacetylenes for Chaihu are useful. The acute toxicity of the ethanol extract of B. longiradiatum and its fractions was also investigated.


Assuntos
Bupleurum/química , Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/análise , Espectrometria de Massas/métodos , Poli-Inos/análise , Animais , Feminino , Modelos Lineares , Masculino , Camundongos , Raízes de Plantas/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
2.
J Pharm Anal ; 1(1): 1-7, 2011 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-29403674

RESUMO

A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill. The chemical profile of the twelve compounds, including geniposidic acid (1), geniposide(2), gentiopicroside(3), liquiritin(4), crocin(5), baicalin(6), wogonoside(7), baicalein(8), glycyrrhizic acid (9), wogonin (10), oroxylin A (11) and aristolochic acid A (12), was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS). The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4. 6 mm, 5 µm) with a gradient solvent system of acetonitrile-0. 1% aqueous formic acid. The validation was carried out and the linearities (r > 0. 9996), repeatability (RSD<1. 8%), intra- and inter-day precision (RSD< 1. 3%), and recoveries (ranging from 96. 6% to 103. 4%) were acceptable. The limits of detection (LOD) of these compounds ranged from 0.29 to 4. 17 ng. Aristolochic acid A, which is the toxic ingredient, was not detected in all the batches of Longdan Xiegan Pill. Furthermore, hierarchical cluster analysis was used to evaluate the variation of the herbal prescription. The proposed method is simple, effective and suitable for the quality control of this traditional Chinese medicine (TCM).

3.
J Nat Prod ; 72(12): 2153-7, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-19994846

RESUMO

Eight new polyacetylenes (1-8) and six known polyacetylenes were isolated from the entire parts of Bupleurum longiradiatum, a poisonous plant. The structures of the new compounds were determined by spectroscopic data interpretation. The absolute configuration of the known compound bupleurotoxin (9) was established by the modified Mosher's method. All isolates were also tested for their cytotoxicity against a human leukemia cell line (HL-60).


Assuntos
Antineoplásicos Fitogênicos/isolamento & purificação , Bupleurum/química , Medicamentos de Ervas Chinesas/isolamento & purificação , Poli-Inos/isolamento & purificação , Alquinos , Antineoplásicos Fitogênicos/química , Antineoplásicos Fitogênicos/farmacologia , Ensaios de Seleção de Medicamentos Antitumorais , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Células HL-60 , Humanos , Estrutura Molecular , Polienos/química , Polienos/isolamento & purificação , Poli-Inos/química , Poli-Inos/farmacologia
4.
Rapid Commun Mass Spectrom ; 23(18): 2903-16, 2009 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-19670339

RESUMO

A high-performance liquid chromatography/electrospray ionization multi-stage tandem mass spectrometry (HPLC/ESI-MS(n)) method was developed to analyze two structurally related groups of Amaryllidaceae alkaloids (AmAs), crinane- and tazettine-type alkaloids, in the species Crinum latifolium and C. asiaticum, as well as different organs of C. latifolium. In ESI-MS(n) spectra of the two types of alkaloids, characteristic fragmentation reactions were observed that allowed us to determine and differentiate them. Based on the fragmentation rules of reference standards, crinane-type alkaloids displayed concurrent neutral loss of C(2)H(5)N (43 u) and C(2)H(6)N (44 u) as well as characteristic ions of m/z 213 and 211, whereas tazettine-type alkaloids exhibited neutral loss of C(3)H(7)N (57 u) [or C(2)H(5)N (43 u), C(3)H(7)NO (73 u)] from the [M+H](+) and [M+H-H(2)O](+) ions. These were supported by quadrupole time-of-flight (Q-Tof)-MS/MS analysis. The chemical complexity of the mixture was resolved by profiling. The compositions of the main crinane- and tazettine-type alkaloids in the above-mentioned species and organs were also compared. Overall, 28 AmAs comprising 14 crinane-type and 14 tazettine-type alkaloids were identified and studied by MS. Among them, 14 AmAs were tentatively characterized from the two species for the first time. This method allowed a rapid analysis of alkaloid distribution and composition of Crinum species, and may also be used for quality control and screening of extracts designated for pharmaceutical application.


Assuntos
Alcaloides de Amaryllidaceae/química , Cromatografia Líquida de Alta Pressão/métodos , Crinum/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Isomerases , Extratos Vegetais/química
5.
J Pharm Biomed Anal ; 49(3): 715-25, 2009 Apr 05.
Artigo em Inglês | MEDLINE | ID: mdl-19201126

RESUMO

Acetophenones in Cynanchum species, especially cynandione A and its derivatives, whose utilization and toxicity in herbal drugs and folk medicines has caused great interest in the chemical investigation, have extensive biological activities. In this paper, a facile method based on high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-ESI-MS(n)) was developed for the analysis of cynandione A derivatives in the roots of the Cynanchum wilfordii and C. auriculatum. ESI-MS/MS and ESI-MS(n) analysis of cynandiones A and B in negative ion mode were firstly performed employing two mass spectrometers each equipped with an ion-trap and a quadrupole time-of-flight (Q-TOF) mass analyzer. The results drawn from both instruments were similar to each other. Characteristic fragmentation pathways were proposed by comparing the spectra of two standards acquired in the experiments. The fragment ions at m/z 283 and 268 were obtained, and then were used as diagnostic ions to screen and identify cynandione A derivatives from the roots of above two species, together with an HPLC-MS(n) method. Total of 28 cynandione A derivatives comprising 4 reported and 24 novel components were identified or tentatively identified. Furthermore, breakdown curves were constructed to distinguish two types of isomers among these compounds. To our knowledge, this is the first report on characterization of acetophenones by HPLC-ESI-MS(n), which allows a rapid and complete analysis of cynandione A derivatives in roots of Cynanchum species.


Assuntos
Acetofenonas/análise , Cynanchum/química , Acetatos , Compostos de Bifenilo/análise , Cromatografia Líquida de Alta Pressão , Indicadores e Reagentes , Isomerismo , Espectroscopia de Ressonância Magnética , Raízes de Plantas/química , Padrões de Referência , Solventes , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
6.
J Pharm Biomed Anal ; 49(4): 1048-55, 2009 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-19201128

RESUMO

A rapid resolution liquid chromatography coupled with evaporative light scattering detection method was established for simultaneous determination of six saikosaponins, namely saikosaponin a, saikosaponin c, saikosaponin d, 6''-O-acetylsaikosaponin a, 3''-O-acetylsaikosaponin d and 6''-O-acetylsaikosaponin d in Bupleurum. The analysis was performed by using an Agilent Zorbax SB-C18 column (1.8 microm, 3.0 mm x 50 mm i.d.) at gradient elution of water and acetonitrile, and the saikosaponins were well separated within 12 min, which provided about a fourfold reduction in analysis time by comparing a conventional high performance liquid chromatography method. Owing to their low ultraviolet absorption, the saikosaponins were detected by evaporative light scattering. The standard curves to quantify the saikosaponins were constructed by the log-log plot, which showed good linearity with the correlation coefficients exceeding 0.9954. The detection limits and quantification limits ranged in 8.38-25.00 microg/mL and 25.13-45.00 microg/mL, respectively. Satisfactory intra-day and inter-day precisions were achieved with the relative standard deviation (R.S.D.) less than 6.58%, and the average recoveries obtained were in the range of 96.9-100.4%. In addition, MeOH-1.0% (v/v) pyridine was found to be the best the extraction solvent when compared to MeOH and MeOH-1.0% (v/v) ammonia water. A total of 23 samples of roots of Bupleurum from different species or locations were examined with this analytical method, and their chemical profiles provided information for the chemotaxonomic investigation. The results demonstrated that the analytical method is highly effective for the quality evaluation of Bupleurum species.


Assuntos
Bupleurum/química , Ácido Oleanólico/análogos & derivados , Saponinas/análise , Cromatografia Líquida de Alta Pressão , Análise por Conglomerados , Luz , Ácido Oleanólico/análise , Raízes de Plantas/química , Padrões de Referência , Reprodutibilidade dos Testes , Espalhamento de Radiação , Solventes , Espectrofotometria Ultravioleta
7.
J Pharm Biomed Anal ; 49(3): 638-45, 2009 Apr 05.
Artigo em Inglês | MEDLINE | ID: mdl-19185441

RESUMO

For quality control purpose, an approach of chemical fingerprinting of Liuwei Dihuang Pill (LDP) and simultaneous determination of its multiple bioactive components were established by using high performance liquid chromatograph (HPLC) coupled with multiple detection techniques. HPLC with ultraviolet detection (HPLC-UV) was used to acquire its fingerprint, and HPLC with combined detections of diode array detector and evaporative light scattering detector (HPLC-DAD-ELSD) was performed to simultaneously determine eight bioactive constituents: including gallic acid, 5-hydroxymethyl furfural, morroniside, sweroside, loganin, paeoniflorin, paeonol and alisol B-23 acetate. The detection limits and quantification limits ranged in 0.11-1.93mug/mL and 0.38-3.85mug/mL, respectively. The validation of the proposed approach was acceptable, with 93.47-104.62% accuracy in recovery test. The intra- and inter-day precisions of the method were evaluated and were less than 3.87%, with accuracy from 95.3% to 103.4%. In addition, the mass spectrometry of the investigated major constituents was also studied. Based on the chromatographic fingerprint data, partial least square (PLS) and discriminate analysis were utilized to visualize the quality information of 60 batches of LDP, and a partial least square-discriminate analysis (PLS-DA) model was constructed with acceptable predictive performance for the discrimination of various products. The proposed approach was expected to be developed as a powerful tool for the quality control of LDP.


Assuntos
Medicamentos de Ervas Chinesas/análise , Cápsulas , Cromatografia Líquida de Alta Pressão , Luz , Controle de Qualidade , Padrões de Referência , Análise de Regressão , Reprodutibilidade dos Testes , Espalhamento de Radiação , Espectrometria de Massas por Ionização por Electrospray , Espectrofotometria Ultravioleta , Comprimidos
8.
J Sep Sci ; 31(18): 3190-201, 2008 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-18763253

RESUMO

A LC-diode array detection (DAD)-ESI-MS/MS method was established for the online characterization and identification of saikosaponins (SSs) from extracts of roots of Bupleurum scorzonerifolium Willd, B. marginatum var. stenophyllum and B. komarovianum. In ESI-MS/MS spectra of SSs, [M-H](- )ions were subjected to the cleavage of glycosidic bonds and produced Y type ions, which can be used to elucidate the structures of saccharide chains and aglycones. Fragmentation of aglycones provided mass information about their major substitutions. For three structural types of SSs, type III can be easily identified by their fragmentation behaviors; while type I and II often occur as isomers and they can be discriminated by their typical UV absorption data. The only sugar ring-cross cleavage corresponding to 76 Da took place at a furanose sugar moiety. As a result, more than 75 SSs, including eight novel compounds, were identified or tentatively characterized based on their UV and mass spectra and retention times. The approach established here allows a comprehensive analysis of the SSs in the genus of Bupleurum and will be helpful for quality control of the crude materials and their related preparations.


Assuntos
Bupleurum/química , Cromatografia Líquida de Alta Pressão/métodos , Ácido Oleanólico/análogos & derivados , Saponinas , Espectrometria de Massas por Ionização por Electrospray/métodos , Medicamentos de Ervas Chinesas/química , Medicina Tradicional Chinesa , Estrutura Molecular , Ácido Oleanólico/química , Ácido Oleanólico/isolamento & purificação , Padrões de Referência , Saponinas/química , Saponinas/isolamento & purificação
9.
Rapid Commun Mass Spectrom ; 21(6): 869-79, 2007.
Artigo em Inglês | MEDLINE | ID: mdl-17294514

RESUMO

Electrospray ionization multi-stage mass spectrometry (ESI-MS(n)) was performed to study the fragmentation behaviour of seventeen steroidal alkaloids (4 protoverine-type alkaloids, 10 germine-type alkaloids and 3 zygadenin-type alkaloids) from the Chinese herb Veratrum nigrum L. The MS(n) spectra of the [M+H](+) ions for steroidal alkaloids provided a wealth of structural information on the substituted groups. In positive ion mode, the three types of alkaloids showed very different characteristic ions: m/z 436 or 418 for protoverine-type alkaloids; m/z 438, 420 or 402 for germine-type alkaloids; m/z 440 or 422 for zygadenin-type alkaloids. These fragments were used to deduce their mass spectral fragmentation mechanisms. Furthermore, the primary compounds in methanolic extracts of the herb of Veratrum nigrum L. were investigated by using liquid chromatography (LC)/ESI-MS(n). As a result, 21 steroidal alkaloids (5 protoverine-type alkaloids, 14 germine-type alkaloids and 2 zygadenin-type alkaloids) were selectively identified from 27 determined peaks. Eleven compounds were unambiguously identified by comparing with standard compounds and ten compounds were tentatively identified or deduced according to their MS(n) data. Two of these compounds (xingangermine and deacetyl xinganveratrine) were found to be novel steroidal alkaloids. In addition, the chemical structures of two pairs of steroidal alkaloid isomers were deduced by comparing their fragment ions. Given the important structural information of known and unknown steroidal alkaloids in crude herbal extracts, this study is useful for identifying these types of steroidal alkaloids in crude materials rapidly and selectively.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Modelos Químicos , Espectrometria de Massas por Ionização por Electrospray/métodos , Esteroides/química , Alcaloides de Veratrum/química , Veratrum/química , Simulação por Computador , Modelos Moleculares
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