RESUMO
Twenty-six batches of Gardeniae Fructus from different producing area were collected for the development of the fingerprint, and the main components of Gardeniae Fructus were identified by liquid chromatography-mass spectrometry. The producing areas of Gardeniae Fructus were distinguished by chemical pattern recognition technology, and the index components of Gardeniae Fructus were quantitated. An UPLC wavelength switching method was adopted, and the separation was carried out on a Waters Acquity UPLC HASS C_(18)(2.1 mm×100 mm, 1.7 µm) column using the mobile phase of acetonitrile-0.5% formic acid water for gradient elution. Principal component analysis(PCA) and orthogonal partial least square discriminant analysis(OPLS-DA) were used for the data ana-lysis. The results showed that the similarity of 26 batches of Gardeniae Fructus was more than 0.89, and ten common peaks were defined. Sixteen compounds including monoterpenes, iridoids and diterpenoids were identified by reference identification, literature comparison and high-resolution mass spectrometry data analysis. The distinguishment of origin of Gardeniae Fructus was realized by PCA and OPLS-DA analysis, and two quality differential markers were screened as geniposide and crocin â . The contents of crocin â , crocin â ¡ and geniposide in Gardeniae Fructus from different places were different. These results will provide reference for the geographical origin traceability of Gardeniae Fructus.
Assuntos
Medicamentos de Ervas Chinesas , Gardenia , Cromatografia Líquida de Alta Pressão , Frutas , Controle de QualidadeRESUMO
The ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS) was used to conduct the qualitative analysis of the monoterpene chemical components from Paeoniae Radix Rubra. Gradient elution was performed on C_(18) HD(2.1 mm×100 mm, 2.5 μm) column with a mobile phase of 0.1% formic acid(A) and acetonitrile(B). The flow rate was 0.4 mL·min~(-1) and the column temperature was 30 ℃. MS analysis was conducted in both positive and negative ionization modes using electrospray ionization(ESI) source. Qualitative Analysis 10.0 was used for data processing. The identification of chemical components was realized by the combination of standard compounds, fragmentation patterns, and mass spectra data reported in the literature. Forty-one monoterpenoids in Paeoniae Radix Rubra extract were identified. Among them, 8 compounds were reported in Paeoniae Radix Rubra for the first time and 1 was presumed to be the new compound 5″-O-methyl-galloylpaeoniflorin or its positional isomer. The method in this study realizes the rapid identification of monoterpenoids from Paeoniae Radix Rubra and provides a material and scientific basis for quality control and further study on the pharmaceutical effect of Paeoniae Radix Rubra.
Assuntos
Cromatografia Líquida , Medicamentos de Ervas Chinesas , Espectrometria de Massas , MonoterpenosRESUMO
Qing-Fei-Pai-Du decoction (QFPDD) is a Chinese medicine compound formula recommended for combating corona virus disease 2019 (COVID-19) by National Health Commission of the People's Republic of China. The latest clinical study showed that early treatment with QFPDD was associated with favorable outcomes for patient recovery, viral shedding, hospital stay, and course of the disease. However, the effective constituents of QFPDD remain unclear. In this study, an UHPLC-Q-Orbitrap HRMS based method was developed to identify the chemical constituents in QFPDD and the absorbed prototypes as well as the metabolites in mice serum and tissues following oral administration of QFPDD. A total of 405 chemicals, including 40 kinds of alkaloids, 162 kinds of flavonoids, 44 kinds of organic acids, 71 kinds of triterpene saponins and 88 kinds of other compounds in the water extract of QFPDD were tentatively identified via comparison with the retention times and MS/MS spectra of the standards or refereed by literature. With the help of the standards and in vitro metabolites, 195 chemical components (including 104 prototypes and 91 metabolites) were identified in mice serum after oral administration of QFPDD. In addition, 165, 177, 112, 120, 44, 53 constituents were identified in the lung, liver, heart, kidney, brain, and spleen of QFPDD-treated mice, respectively. These findings provided key information and guidance for further investigation on the pharmacologically active substances and clinical applications of QFPDD.
Assuntos
Animais , Camundongos , Administração Oral , Alcaloides/análise , COVID-19 , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/farmacocinética , Flavonoides/análise , SARS-CoV-2 , Saponinas/análise , Triterpenos/análiseRESUMO
A simple and fast capillary gas chromatographic (CGC) method with flame ionization detection is developed for the analysis of fatty oil in Semen Ziziphi Spinosae. After methyl-esterification, eight components are identified by gas chromatography-mass spectrometry. The derivatization condition is investigated in order to validate this method. Palmitic acid and stearic acid are quantitated simultaneously. The limits of detection are 5.024 microg/mL for palmitic acid and 6.957 microg/mL for stearic acid, respectively. The limits of quantitation are 16.76 microg/mL for palmitic acid and 23.19 microg/mL for stearic acid, respectively. The percent recoveries of palmitic and stearic acid are 97.4% and 96.6%. CGC is shown to be a quick and informative tool for the analysis of fatty oil in Semen Ziziphi Spinosae.
Assuntos
Cromatografia Gasosa/métodos , Ácidos Graxos/análise , Óleos de Plantas/análise , Sementes/química , Ziziphus/embriologia , Reprodutibilidade dos Testes , Sensibilidade e EspecificidadeRESUMO
<p><b>OBJECTIVE</b>To provide experimental data for the quality control of processed Paeonia lactiflora, a Chinese herbal medicine.</p><p><b>METHOD</b>Traditional processing of P. lactiflora was simulated, content of paeoniflorin and water extracts among different preparations were assayed by HPLC; The quantitative correlations among different processing conditions were analyzed, the effects of processing parameters on the contents of paeoniflorin and water extracts were assayed and analysed.</p><p><b>RESULT AND CONCLUSION</b>The controlled processing parameters were correlated with covariables which showed that processing procedures was controllable, and the heating temperature was a factor impacting the content of paeoniflorin.</p>
Assuntos
Ácidos Cafeicos , China , Cromatografia Líquida de Alta Pressão , Métodos , Ecossistema , Lycopus , Química , Componentes Aéreos da Planta , Química , Plantas Medicinais , Química , Controle de Qualidade , Reprodutibilidade dos Testes , Estações do Ano , Sensibilidade e EspecificidadeRESUMO
<p><b>AIM</b>To analyze the chemical components in Danggui (the roots of Angelica sinensis (Oliv.) Diel).</p><p><b>METHODS</b>HPLC-MS/MS was used to identify the main components in Danggui. Furthermore, the MS fragmentation regularity of the phthalides was proposed. The mobile phase of HPLC consisted of 0.5% acetic acid in water and 0.5% acetic acid in acetonitrile, analytical column was Hypersil ODS2 (250 mm x 4.6 mm, 5 microm), flow rate 1.0 mL x min(-1), injected volume 2 microL. The ionization source was ESI in positive ion mode.</p><p><b>RESULTS</b>Ferulic acid, nine known phthalides and one unknown phthalide derivative were tentatively identified in chromatograms based on their MS data and the comparison of their UV spectra with those published in the literatures.</p><p><b>CONCLUSION</b>The structural information of phthalides was obtained via HPLC-MS/MS, which provides an accurate and fast method to identify the phthalides and provides more scientific information for quality control of Danggui.</p>
Assuntos
4-Butirolactona , Química , Angelica sinensis , Química , Benzofuranos , Química , Cromatografia Líquida de Alta Pressão , Métodos , Ácidos Cumáricos , Química , Estrutura Molecular , Anidridos Ftálicos , Química , Raízes de Plantas , Química , Plantas Medicinais , Química , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray , MétodosRESUMO
<p><b>AIM</b>To evaluate the similarity between two chromatographic fingerprints automatically with computer.</p><p><b>METHODS</b>Chromatogram can be treated as vector of hyperspace, and the similarity between them can be counted according to vectorial angle formula. This process was performed with software written in Visual Basic 6.0. The two main functions of this software are automatic peak tracking in two fingerprints under the same analytic condition and computing the similarity automatically.</p><p><b>RESULTS</b>The HPLC fingerprints of eleven kinds of Evodia rutaecarpa (Juss.) Benth (a traditional Chinese herb) from different sources were obtained and the similarities were calculated with this software. This method was shown to be a good way to evaluate the similarity between two fingerprints. A sample washed seven times with hot water can be clearly discriminated from other samples of Evodia rutaecarpa (Juss.) Benth with similar results.</p><p><b>CONCLUSION</b>This method is a good way to evaluate the similarity between two fingerprints and is helpful in quality control of traditional Chinese medicine.</p>
Assuntos
Evodia , Química , Classificação , Plantas Medicinais , Química , Controle de Qualidade , Design de SoftwareRESUMO
<p><b>AIM</b>To study the pharmacokinetics of spinosin in rat plasma after oral administration of Suanzaoren extract using sulfamethoxazole (SMZ) as internal standard by RP-HPLC method.</p><p><b>METHODS</b>Plasma samples were deproteined with acetonitrile, followed by evaporation of the acetonitrile to dryness. The residual was then resolved in mobile phase and HPLC separation was achieved on a Hypersil C18 (5 microns, 200 mm x 4.6 mm ID) column at 35 degrees C. The mobile phase consisted of acetonitrile-water-acetic acid (15:85:1) at a flow rate of 0.7 mL.min-1. The UV detection wavelength was set at 334 nm.</p><p><b>RESULTS</b>The calibration curve was shown to be linear over the range from 18.1 to 903.5 micrograms.L-1 (r2 > or = 0.995). Mean recovery was 94.5%. Within-day and between-day precisions RSD were less than 9.0%. The limit of quantitation was 18.1 micrograms.L-1. The plasma spinosin was stable at -20 degrees C.</p><p><b>CONCLUSION</b>The simple, sensitive and accurate HPLC method developed has been applied to determine the pharmacokinetics of spinosin in rat plasma after having taken Suanzaoren extract at a single dose.</p>
Assuntos
Animais , Ratos , Administração Oral , Cromatografia Líquida de Alta Pressão , Métodos , Medicamentos de Ervas Chinesas , Farmacocinética , Flavonoides , Sangue , Farmacocinética , Plantas Medicinais , Química , Ratos Wistar , Sementes , Química , Ziziphus , QuímicaRESUMO
<p><b>OBJECTIVE</b>To establish a method for GC fingerprint determination of the chemical constituents in Herba Asari.</p><p><b>METHOD</b>GC and GC-MS were used to optimize the fingerprint determination method, and identify the main peaks in the GC fingerprint.</p><p><b>RESULT</b>A preferable method for GC fingerprint determination of the chemical constituents in Herba Asari was established.</p><p><b>CONCLUSION</b>A general acquaintance of the chemical constituents in Herba Asari can be obtained by using the preferable GC fingerprint determination method, which is useful for quality evaluation of the crude drug of Herba Asari.</p>