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Chronic inflammation results from excessive pro-inflammatory signaling and the failure to resolve the inflammatory reaction. Lipid mediators orchestrate both the initiation and resolution of inflammation. Switching from pro-inflammatory to pro-resolving lipid mediator biosynthesis is considered as efficient strategy to relieve chronic inflammation, though drug candidates exhibiting such features are unknown. Starting from a library of Vietnamese medical plant extracts, we identified isomers of the biflavanoid 8-methylsocotrin-4'-ol from
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OBJECTIVE: To establish a rapid ultra-high performance liquid chromatography method for determining teicoplanin concentration in human plasma. METHODS: The samples were chromatographed on Waters Acquity UPLC BEH-C18 column using gradient elution method(mobile phase A:20 mmol•L-1 ammonium acetate;mobile phase B:acetonitrile). The absorption wavelength was set at 215 nm. The column temperature were maintained at 35 ℃. The teicoplanin concentration was calculated by internal standard method and external standard method, respectively. The results of the two methods were compared by paired t-test using SPSS statisticals software. RESULTS: The liner range of the calibration curve for teicoplanin was 3.15-100 μg•mL-1(r=0.999 9). The concentrations calculated by the two methods had good correlation without significant difference. CONCLUSION: This method is proved to be rapid, sensitive and suitable for the therapeutic drug monitoring and pharmacokinetic investigation of teicoplanin in human plasma.
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Se presentan en este artículo los resultados del desarrollo y validación de una metodología analítica para la cuantificación de Candesartan Cilexetil en tabletas recubiertas para uso humano. El procedimiento consiste en una separación por cromatografía líquida de alta eficiencia en fase inversa y detector de arreglo de diodos, empleando como fase móvil una mezcla compuesta por un buffer de acetatos de pH 4,0 y acetonitrilo (30:70), una columna C18 a temperatura ambiente y detección a una longitud de onda de 306 nm. Se comprobó la selectividad, la precisión y la exactitud de la metodología. Estas características junto con su sencillez hacen el método adecuado y conveniente para el objetivo propuesto. La robustez de la metodología se investigó frente a la variación de algunas de las condiciones cromatográficas bajo las cuales se llevó a cabo la validación.
A reverse phase high performance liquid chromatographic method was developed for the quantitative assay of candesartan ciletexil in coated tablets for human use as hypotensor agent. The method was then validated for its quantitative determination assay in tablets as pharmaceutical specialties. A C18 column stabilized at room temperature was used and the detection was performed at 306 nm. A mixture of acetonitrile, acetate buffer pH 4,0 (30:70) was used as the mobile phase. The method is selective, linear and shows a good repeatability. The robustness was also studied. These properties besides the simplicity make the methodology convenient for the objective proposed.
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OBJECTIVE: To establish a rapid column-switching-ultra high performance liquid chromatography method for determining meropenem concentration in human plasma. METHODS: Meropenem plasma samples were diluted by internal standard aqueous solution (doxofylline), filtrated by microporous membrane, and then extracted by on-line column-switching method. The samples were chromatographed on Waters Acquity UPLC@BEH-C18 column using gradient elution method (mobile phase A and extracting mobile phase C: methanol -0.05 mol·L-1 K2HPO4 (pH 7.0) 5:95; mobile phase B: methanol). The maximum absorption wavelength of meropenem was 299 nm. The column temperature were 35°C. The meropenem concentration was calculated by internal standard method and external standard method, respectively. The results of the two methods were compared by paired t-test using SPSS statistical software. RESULTS: The liner range of the calibration curve for meropenem was 0.67-86.00 mg·L-1 (r=0.9999). The method recovery was (93.59±1.15)%-(99.21±4.06)% and extraction recovery was above 85.0%, relative standard deviation was below 5.0%. The SPSS statistic results indicated there was no significant difference between the concentrations calculated by the two methods and existed good correlation. The transformed equation is ρInternal=1.039ρExternal-0.468 (r=0.9970). CONCLUSION: On-line column-switching method is used and it is proved to be rapid, sensitive and suitable for therapeutic drug monitoring and pharmacokinetic investigation of meropenem in human plasma.
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Objective: To develop a quantitative analysis of multi-components by single-marker (QAMS) method for the simultaneous determination of eight components in Astragali Radix products, and to examine the feasibility of using the method among the different dosage forms and between two different types of compounds. Methods: Eight main effective components, campanulin, genistin, ononin, calycosin, genistein, formononetin, methylnissolin, and astragaloside IV were selected as analytes for the quality control of Astragali Radix products. Calycosin was selected as the internal reference substance, the content of which was determined by external standard method; the relative correction factors (RCFs) of campanulin, genistin, ononin, genistein, formononetin, methylnissolin, and astragaloside IV were calculated. In total, twelve Astragali Radix specimen in decoction pieces, as well as in two different dosage forms, such as granule and oral liquid products, were used for the quality control by both methods of external standard and QAMS. The validity of the QAMS method was evaluated by comparison on the quantitative results of the two methods. Results: These RCFs were obtained with good reproducibility (RSD < 6.5%) by using ultra high performance liquid chromatography coupled with diode array detector under various chromatographic conditions. Meanwhile, no obvious differences (RSD < 3.98%) were found in the quantitative results of the seven components in twelve samples of Astragali Radix products determined by the two methods. Conclusion: QAMS is a reliable and feasible method in determining the components in products of Astragali Radix. © 2013 Tianjin Press of Chinese Herbal Medicines.
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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).
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A simple and accurate high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD) and evaporative light scattering detector (ELSD) was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation (ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis (HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.
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A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.
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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）.
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A method for the determination of bisphenol A, octyphenol, nonylphenol in water samples was developed using stir bar sorptive extraction (SBSE) based on poly (vinylimidazole-divinylbenzene) monolithic material (SBSEM) combined with high performance liquid chromatography with diode array detection.To achieve the optimum extraction performance, several main extraction parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated.Under the optimized experimental conditions, the method showed good linearity and repeatability, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.13-0.66 and 0.44-2.19 μg/L, respectively.The extraction performance of SBSEM to the target compounds was also compared with commercial SBSE which used polydimethylsiloxane as coating.The proposed method was successfully applied to the determination of the target compounds in water samples.The recoveries of spiked target compounds in real samples ranged from 37.8%-101.1%.The results indicated that the developed method possessed advantages such as sensitivity, simplicity, low cost and high feasibility.
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Microwave-assisted extraction (MAE) was used for extraction of effective components of sarcandra glabra (Thunb.), and then chromatographic fingerprint of sarcandra glabra (Thunb.) was studied by high performance liquid chromatography/diode array detector (HPLC/DAD). The conditions of MAE were optimized by an orthogonal experiment, and then the authentication and validation of the chromatographic fingerprint were conducted. Nine peaks were identified as common peaks in the fingerprint chromatograms, and isofraxidin was considered as a reference compound and quantified. Relative standard deviations of retention time and peak area of each component were less than 3 % and 8 %, respectively. Similarity and difference analysis were conducted by use of PCA and relation coefficient. Twenty batches of sarcandra glabra (Thunb.) samples from two different producing areas could be classified into two different groups in the PCA model. The results showed that MAE-HPLC/DAD method was simple, efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra (Thunb.), which could provide more reliable and precise information for quality evaluation.
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Microwave-assisted extraction (MAE) was used for extraction of effective components of sarcandra glabra (Thunb.), and then chromatographic fingerprint of sarcandra glabra (Thunb.) was studied by high performance liquid chromatography/diode array detector (HPLC/DAD). The conditions of MAE were optimized by an orthogonal experiment, and then the authentication and validation of the chromatographic fingerprint were conducted. Nine peaks were identified as common peaks in the fingerprint chromatograms, and isofraxidin was considered as a reference compound and quantified. Relative standard deviations of retention time and peak area of each component were less than 3% and 8%, respectively. Similarity and difference analysis were conducted by use of PCA and relation coefficient. Twenty batches of sarcandra glabra (Thunb.) samples from two different producing areas could be classified into two different groups in the PCA model. The results showed that MAE-HPLC/DAD method was simple, efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra (Thunb.), which could provide more reliable and precise information for quality evaluation.
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OBJECTIVE:To develop an HPLC method for determination of main component in low concentration of alprostadil for injection. METHODS: Diode array detector was used for full wavelength scanning of the low concentration of alprostadil sample solution (20 ?g?mL-1) with detection wavelength set at 214 nm and the reference wavelength at 250 nm. The mobile phase consisted of acetonitrile-0.02 mol?L-1 KH2PO4 solution (pH 4.9,40∶60) at a flow rate of 1 mL?min-1. RESULTS: The linear range of alprostadil was 10～320 ?g?mL-1 (r=0.999 9) and the average recovery rate was 98.26% (RSD=1.68%). CONCLUSION: The method is of low cost and it is applicable for the determination of the low concentration of alprostadil for injection.
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OBJECTIVE:To develop a HPLC assay for the determination of 7 kinds of amino acids in amino acid capsules by using online derivation and diode array detector.METHODS:The high performance chromatograph of liquid with the device of automatic derivation was employed as the automatic sampler.The samples were injected in the predefined procedure,and detected with the diode array detector.RESULTS:Good resolution of 7 kinds of amino acids was obtained,and the respective detectable concentration showed a good linear relationship with its peak area.CONCLUSION:The present method is convenient,well reproduced, highly sensitive,and accurate,therefore it can be widely used.