Poly-ε-caprolactone based nanoparticles for delivery of genistein in melanoma treatment

We developed poly-ε-caprolactone (PCL)-based nanoparticles containing D-α-tocopherol polyethylene glycol-1000 succinate (TPGS) or Poloxamer 407 as stabilizers to efficiently encapsulate genistein (GN). Two formulations, referred to as PNTPGS and PNPol, were prepared using nanoprecipitation. They were characterized by size and PDI distribution, zeta potential, nanoparticle tracking analysis (NTA), GN association (AE%), infrared spectroscopy (FT-IR), and differential scanning calorimetry (DSC). PNTPGS-GN exhibited a particle size of 141.2 nm, a PDI of 0.189, a zeta potential of -32.9 mV, and an AE% of 77.95%. PNPol-GN had a size of 146.3 nm, a better PDI than PNTPGS-GN (0.150), a less negative zeta potential (-21.0 mV), and an AE% of 68.73%. Thermal and spectrometric analyses indicated that no new compounds were formed, and there was no incompatibility detected in the formulations. Cellular studies revealed that Poloxamer 407 conferred less toxicity to PCL nanoparticles. However, the percentage of uptake decreased compared to the use of TPGS, which exhibited almost 80% cellular uptake. This study contributes to the investigation of stabilizers capable of conferring stability to PCL nanoparticles efficiently encapsulating GN. Thus, the PCL nanoparticle proposed here is an innovative nanomedicine for melanoma therapy and represents a strong candidate for specific pre-clinical and in vivo studie

Qualitative and quantitative study of constituents in Lysionoti Herba based on UHPLC-Q-Exactive Orbitrap HRMS and HPLC-UV / 中国中药杂志

Ultra-high performance liquid chromatography-quadrupole-Exactive Orbitrap high resolution mass spectrometry(UHPLC-Q-Exactive Orbitrap HRMS) was employed to systematically analyze the chemical constituents in Lysionoti Herba, and high perfor-mance liquid chromatography-ultraviolet(HPLC-UV) to determine the content of main compounds. A Synergi~(TM) Hydro-RP 100 Å colu-mn(2 mm×100 mm, 2.5 μm) was used for gradient elution with acetonitrile-0.1% aqueous formic acid as the mobile phase at a flow rate of 0.2 mL·min~(-1) and a column temperature of 40 ℃. MS and MS/MS were conducted with electrospray ionization(ESI) in both positive and negative modes. The chemical components in Lysionoti Herba were identified by comparison with the retention time and mass spectra of reference compounds and the relevant mass spectral data reported in MS databases and relevant literature. Furthermore, the content of five constituents(neochlorogenic acid, chlorogenic acid, forsythoside B, acteoside, and nevadensin) in different Lysiono-ti Herba samples was simultaneously determined by HPLC-UV at the wavelength of 330 nm. A total of 84 compounds were identified in Lysionoti Herba, including 27 flavonoids, 20 phenylethanoid glycosides, 5 amino acids, 18 organic acids, 1 alkaloid, 6 nucleosides, and 7 others. The content of neochlorogenic acid, chlorogenic acid, forsythoside B, acteoside, and nevadensin showed good linear relationship(r>0.999) with the peak area within certain concentration ranges, which were 3.22-102.90, 12.84-410.82, 31.63-1 012.01, 25.00-800.11, and 4.08-130.51 μg·mL~(-1), respectively. The instrument precision, method repeatability, and solution stability all met requirement, and the average recovery rate was 97.31%-100.2%, with RSD ranging from 0.95% to 2.4%. The content of the five components varied among different Lysionoti Herba samples collected from different regions of Guizhou, and the average content of forsythoside B was the highest. The established qualitative method can rapidly and efficiently identify the chemical components of Lysionoti Herba, and the developed HPLC-UV method can simultaneously determine the content of five components in a simple, ra-pid, and accurate manner, providing a scientific basis for the quality evaluation of Lysionoti Herba.

Preservation of phenolic compounds on dried leaf infusion of Bauhinia forficata Link

Abstract Bauhinia forficata Link aqueous extract is usually recommended as a phytomedicine to reduce blood glucose levels and its biological activity has been linked to the presence of phenolic compounds from B. forficata preparations. Several drying processes are used in the production of dry herbal extracts, which may influence the chemical composition and efficacy of final herbal medicines. Due to significant chemical changes, defining appropriate drying processes is essential for phytopharmaceutical drug development. In view of this, we analyzed dried B. forficata leaf infusion (BFLI) extracts by HPLC-UV-MSn, followed by molecular networking analysis to evaluate the chemical profiles from dried extracts yielded by freeze-and spray-drying processes. The main metabolites detected included 11 ferulic/isoferulic acid derivatives and 13 glycosylated flavonoids. The qualitative chemical profiles were alike for both drying processes, whereas the relative abundance of some flavonoids was higher using spray-drying. Taken together, our results showed that freeze-and spray-drying preserved the phenolic profile of BFLI and suggested that spray-drying may be the most suitable to obtain its dried products. Along with studying the chemical profiles of dried herbal extracts, evaluating the influence of drying processes on the quality and chemical profiles of final products is pivotal and may benefit future research.

Determination of sunset yellow, allura red, and fast green using a novel magnetic nanoadsorbent modified with Elaeagnus angustifolia based on magnetic solid-phase extraction by HPLC

Abstract Sunset yellow (SY), allura red (AR) and fast green (FG) are frequently used in commercial food products, although they are considered to be hazardous to public health due to their toxic efficacy and high exposure risk potency. In this study, a new, rapid, and reliable method based on a magnetic solid-phase extraction (MSPE) was developed for the simultaneous determination of SY, AR, and FG. Fe3O4 modified with Elaeagnus angustifolia was used for the first time as an adsorbent (Fe3O4-EA) in MSPE. It was characterized with scanning electron microscopy, Brunauer Emmet Teller surface area analysis and X-ray diffraction. MSPE parameters were optimized in terms of pH, adsorption, and elution time and elution volume. High-performance liquid chromatography was used for dye quantitation. Analytical separation was performed by applying ammonium acetate buffer, acetonitrile, and methanol as the mobile phase to a C18 reverse-phase analytical column. Intraday and inter-day repeatability of the method performed at the concentration of 0.2, 1.0 and 2.0 µg/mL exhibited <8.1% RSD (n=3). The limit of detection values was between 0.05-0.1 µg/mL. The adsorption data of SY, AR and FG on Fe3O4-EA were fitted with the Langmuir model with qmax values of 45.0, 70.4 and 73.0 mg/g, respectively.

Pharmacokinetic comparison with different assays for simultaneous determination of cis-,trans-cefprozil diastereomers in human plasma / 药物分析学报

The purpose of this study was to compare pharmacokinetic (PK) parameters obtained using two newly developed assays,HPLC-UV and UPLC-ESI-MS/MS.Selection of assay and results obtained therefrom are very important in PK studies and can have a major impact on the PK-based clinical dose and usage settings.For this study,we developed two new methods that are most commonly used in biosample analysis and focused on PK parameters obtained from them.By HPLC-UV equipped with a Luna-C8 column using UV detector,cefprozil diastereomers were separated using water containing 2％ (V/V) acetic acid and acetonitrile as a mobile phase.By UPLC-ESI-MS/MS equipped with a HALO-C18column,cefprozil diastereomers were separated using 0.5％ (V/V) aqueous formic acid containing 5 mM ammonium-formate buffer and methanol as a mobile phase.Chromatograms showed high resolution,sensitivity,and selectivity without interference by plasma constituents.Both intra-and inter-day precisions (CV,％)were within 8.88％ for HPLC-UV and UPLC-ESI-MS/MS.Accuracy of both methods was 95.67％-107.50％.These two analytical methods satisfied the criteria of international guidance and could be successfully applied to PK study.Comparison of PK parameters between two assays confirmed that there is a dif-ference in the predicted minimum plasma concentrations at steady state,which may affect clinical dose and usage settings.Furthermore,we confirmed possible correlation between PK parameters and various biochemical parameters after oral administration of 1000 mg cefprozil to humans.

Rapid Screening and Identification of Antioxidant Active Components in Glycyrrhiza uralensis Decoction Pieces / 中国药房

OBJECTIVE：To establish a method for online detection of antioxidant active components in Glycyrrhiza uroalensis decoction pieces ，and to identify it. METHODS ：The free radical scavenging rate of 1，1-diphenyl-2-trinitrobenzene hydrazine （DPPH）was determined to evaluate the antioxidant activity of G. uralensis decoction pieces. HPLC-UV-DPPH method was used to screen the anti oxidant active components of G. uralensis decoction pieces. HPLC-TOF/MS was used to obtain mass spectrum data and Qualitive Analyst B 06.00 Build 6.0.633.0 software was used to analyze data. Through contrast analysis of UV absorption spectrum，online chromatogram ，mass spectrum information of G. uralensis and the retention time of each compound ，accurate molecular weight ，antioxidant active components were identified by referring to relevant literature. Validation test was also conducted. RESULTS ：DPPH free radical scavenging rate in 8 batches of G. uralensis decoction pieces ranged 55.71％-60.17％. Seven antioxidative active compounds ，including avolomotor ，8-isopentenyl naringin ，yellow lupulin weitone ，isoflavone B ，3′， 4′-dimethoxy3-hydroxy-6-methyl flavone ，glycyrrhizin E and glycyrrhizin H ，could be screened from G. uralensis decoction pieces. After validation ，the peak area of inverted peak generated by online reaction was positively correlated with DPPH free radical scavenging rate. CONCLUSIONS ：Established method is simple and accurate ，and can be used to quickly screen and identify the main antioxidant components of G. uralensis decoction pieces ；the peak area of inverted peak can be used to evaluate the antioxidant active components of G. uralensis decoction pieces.

Pharmacokinetics and tissue distribution characteristics of sunitinib / 中国临床药理学与治疗学

AIM: To establish a HPLC-UV method to determine sunitinib in rat plasma and mouse tissues, and to study its pharmacokinetics in rats and tissue distribution characteristics in mice. METHODS: The biotic samples were prepared by protein precipitation followed by a stereoselective analysis of sunitinib was achieved on Waters XBridgeTM C18 (4.6 mm×250 mm, 5 μm) with a mobile phase composing of methanol-0.02 mol/L sodium dihydrogen phosphate (70:30) at a flow rate of 1.0 mL/min. The detection wavelength was 310 nm, and the column temperature was 25 ℃. RESULTS: The calibration curve for rat plasma sunitinib was linear in the range of 0.019 2-15.34 μg/mL. The linear ranges in mice brain and kidney were 0.038 3-11.50 and 0.038 3-69.00 μg/mL, respectively. After intragastric administration of sunitinib at a dose of 20 mg/kg to rats, the pharmacokinetic characteristics were Tmax=9.0 h, Cmax=0.194 mg/L, t1/2=18.4 h, AUC(0-∞)=6.8 mg•L-1•h. And the absolute bioavailablity was 47.1%. It was indicated that sunitinib could permeate the blood brain barrier, but the concentration was lower in brain and higher in kidney. CONCLUSION: A HPLC-UV method for the determination of sunitinib in rat plasma and mouse tissues was established. The method is simple, rapid, reliable, and provides a reference for the clinical application of sunitinib.

Quantitative analysis of phenobarbital in biological fluids: Analyte enrichment by an electrically-assisted microextraction technique

An electrically-assisted microextraction method called electromembrane extraction, followed by a simple high performance liquid chromatography and ultraviolet detection was developed and validated for determining phenobarbital in biological samples. The major parameters influencing the electromembrane extraction procedure including solvent composition, voltage, pH of acceptor and donor solutions, salt effect, and time of extraction were evaluated and optimized. The drug was extracted from the donor aqueous sample solution (pH 9) to the acceptor aqueous solution (pH 13). The donor and acceptor phases were separated by a hollow fiber dipped in 1-octanol as a supported liquid membrane. A voltage of 40 V during 20 minutes was applied as the driving force. The enrichment factor was obtained >51 which enhanced the sensitivity of the instrument. Limit of detection and limit of quantitation were 7.5 and 25 ng/mL, respectively. The method was linear over the range of 25-1000 ng/mL for phenobarbital (R2 >0.9998) with repeatability (%RSD) between 0.4% and 6.8% (n = 3). The proposed method was successfully applied to human plasma and urine samples with relative recovery of 70-80% and %RSD < 6.8%.

Chemical composition of propolis extract and its effects on epirubicin-induced hepatotoxicity in rats

ABSTRACT Propolis is a natural substance, produced by honeybees from the resin of various plants. The purpose of this study was to determine the chemical composition and evaluate the hepatoprotective effect of ethyl acetate extract of propolis from Tigzirt, against the toxicity induced by epirubicin which is a anticancer agent, and belongs to the family of antracyclines. The study included thirty male Wistar albino rats divided into five groups. The rats received the extraction of propolis or the quercetin orally for 15 days. The hepatotoxicity was promoted by injection epirubicin (i.v.) with a cumulative dose of 9 mg/kg. Several biological parameters were measured. Oxidative status was also assessed by evaluating antioxidant enzyme and histological study of some organs. Epirubicin caused oxidative stress by a significant decrease in hepatic antioxidant enzymes (gluthation peroxidase, catalase, superoxide dismutase), increased malondialdehyde and liver parameters (ASAT, ALAT, γGT, ALP) compared to the control. The histological study revealed major damage to the liver. Perturbations in this liver function, antioxidant status and damage to the liver by epirubicin have been repaired by the administration of propolis. Furthermore, epirubicin showed inflammatory effects induced by an increase in TNF-α and PGE2. Pretreatment with propolis to rats restored these inflammatory parameters. The chemical identification of extract of propolis by HPLC/UV shows the presence of polyphenolic compounds and many flavonoids. The propolis extract showed a significant reduction in oxidative damage from oxidative stress and a very important protective effect against epirubicin-induced hepatotoxicity.

HPLC profile and simultaneous quantitative analysis of tingenone and pristimerin in four Celastraceae species using HPLC-UV-DAD-MS

ABSTRACT A validated method for the identification and authentication of tingenone and pristimerin was developed using HPLC. The chromatographic profile analysis was combined with simultaneous quantification in Crossopetalum rhacoma Crantz, Cassine xylocarpa Vent, Semialarium mexicanum (Miers) Mennega (known as cancerina), and Maytenus phyllanthoides Benth, through microwave-assisted extraction. The HPLC profiles of the four analyzed species showed three similar signals, which corresponded to the main chemotaxonomic markers of the Celastraceae family: quinonemethide triterpenes. HPLC profile analysis was used as a tool to identify the relationship with the quinonemethide triterpenes, for establishing the taxonomic position of some species whose placement in, or within, the Celastraceae family is uncertain.

Screening of anti-oxidant components of Gongcheng Tea by HPLC-UV-FLD and micro-injection systems / 中草药

Objective: A high performance liquid chromatography-ultraviolet-fluorescence (HPLC-UV-FLD) derivative system was established and the anti-oxidant activity of the extract of Gongcheng Tea was preliminarily evaluated by using a micro-injector imaging system combined with a fluorescent probe. Methods: Hydrogen peroxide assay and hydroxyl radical scavenging ability experiments were carried out on the anti-oxidant activity of Gongcheng Tea. The anti-oxidant components of Gongcheng Tea were screened by HPLC-UV-FLD post column derivation system and analyzed by an ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q/TOF MS). At the same time, the hydrogen peroxide scavenging activity of tea and active components were tested by a micro-injector imaging system combined with a hydrogen peroxide fluorescent probe (NBCD) in living Drosophila melanogaster. Results: The method was simple and rapid, and three main anti-oxidant compounds, epigallocatechin, epigallocatechin gallate, and epicatechin gallate were found in Gongcheng Tea. And it was found that they could significantly reduce the level of hydrogen peroxide in D. melanogaster. Conclusion: It laid a material basis for the further study of the anti-oxidant activity of Gongcheng Tea, and provided a reference for the screening of anti-oxidants in natural products.

Evaluation of scavenging activity of hydrogen peroxide in different origins of Liropes Radix by HPLC-UV-CL system / 中国中药杂志

The hydrogen peroxide generation system was used to analyze the scavenging activity of hydrogen peroxide by Liropes Radix from different origins by HPLC-UV-CL. The UV-CL fingerprints of Liropes Radix from different origins were evaluated,and the HPLC-UV and LC-CL fingerprints were systematically analyzed and evaluated. The results showed that the ether fractions of Liriope spicata var. prolifera and L. muscari had good scavenging activity of hydrogen peroxide,and the total activity of different origins varied greatly,while the similar samples had similar activities. The total antioxidant activity of L. muscari is higher than that of L. spicata var.prolifera. The similarity analysis of the two fingerprints was carried out by two different analytical methods. The chemical fingerprints and the active fingerprints have different characteristics. The contribution of each fingerprint to the total peak area and total activity is also different. There are significant differences between the two different fingerprint clustering results.

Quality Evaluation and Identification of Phyllanthi Fructus at Different Storage Years Based on HPLC-UV and FT-NIR / 中国实验方剂学杂志

Objective: To explore the change rules of active ingredients in Phyllanthi Fructus of different storage years,in order to provide theory basis for storage. Method: Seven Phyllanthi Fruatus samples of different storage years were collected. HPLC-UV detection method was established to determine the contents of gallic acid,corilagin,chebulagic acid,ellagic acid and quercetin. Samples were fingerprinted by FT-NIR and identified by PLS-DA model. Result: Gallic acid,which was the bioactive marker in Chinese Pharmacopoeia,had the highest content. It was followed by ellagic acid and chebulagic acid,and corilagin and quercetin had the least content. The components had significant differences between samples of different storage years (P-1 respectively. The contents of chebulagic acid,corilagin and ellagic acid reached a maximum at 4 years of storage,which were 18.85,7.97,21.46 mg·g-1,respectively. FT-NIR data was optimized by MSC+SG (second derivative, the window parameter as 11,and the polynomial order as 3). The classification accuracy was 84.5%. Spectral data reduced to several important potential variables,and was fused with 5 active components based on minimum cross-validation root mean square error,and the classification accuracy increased to 98.8%. Conclusion: The analysis of PLS-DA by HPLC-UV and FT-NIR could effectively explain the accumulation characteristics of active components in Phyllanthi Fruatus. According to the data fusion strategy,PLS-DA model could distinguish samples of different qualities. The results provide a scientific basis for the quality evaluation and identification of Phyllanthi Fruatus.

Qualitative and quantitative analyses of Chrysanthemum morifolium ‘Fubaiju’ by LC-MSn and HPLC-UV / 中国药科大学学报

@#A qualitative analytical method of liquid chromatography coupled with mass spectrometry(LC-MSn)was developed for the identification of main constituents in Chrysanthemum morifolium ‘Fubaiju’. High-performance liquid chromatography(HPLC)was developed for the quantification of five active components, including chlorogenic acid(1), luteolin-7-O-β-D-glucopyranoside(2), luteolin-7-O-β-D-glucopyranuronide(3), 3, 5-Di-caffeoylquinic acid(4), and apigenin-7-O-β-D-glucopyranoside(5). A total of 22 compounds, including 13 flavonoids and 9 phenolic acids, were identified based on their retention behaviors, UV profiles and MS fragment information. Furthermore, a validation method with good linearity(r> 0. 999 9), precision, stability, repeatability and recovery was successfully applied for simultaneous determination of five major components in 10 batches of C. morifolium ‘Fubaiju’ by HPLC-UV method. The established method was proved to be a validation strategy for the quality evaluation of C. morifolium ‘Fubaiju’.

Assessment of the Purity of Emodin by Quantitative Nuclear Magnetic Resonance Spectroscopy and Mass Balance

Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

Some triterpenic compounds in extracts of Cecropia and Bauhinia species for different sampling years

ABSTRACT The aim of this paper is to provide an overview on the chemical composition of triterpenes in widespread used folk medicine species, through the development and validation of eleven compounds using HPLC-UV detection. The compounds were separated using isocratic elution, on a reverse phase column (Kinetex C18, 250 mm × 4.6 mm, 5 µm) with mobile phase consisted of acetonitrile:tetrahydrofuran (90:10, v/v), flow-rate of 0.5 ml/min and detection in 210 nm. Diverse validation parameters were successfully evaluated. The samples of Bauhinia variegata L., B. variegata var. candida Voigt, Fabaceae, Cecropia palmata Willd. and C. obtusa Trécul, Urticaceae, collected in 2012, 2013 and 2014 from Amazon were treated with two different solvents (ethyl acetate and chloroform) and analyzed by the proposed method. Stigmasterol, lupeol, β-sitosterol, β-amirin and α-amirin were found in all the studied plants. Highlighting the presence of oleanolic acid, maslinic acid in C. obtusa and C. palmata extracts, erythrodiol only in C. palmata, stigmasteol in B. variegata and α-amirin in B. variegata var. candida. Overall, ethyl acetate showed better performance as the extractor solvent than chloroform. Moreover, it could be used for the quality control of medicinal plants and to assess potential marker compounds.

Study of anti-oxidants of Rehmanniae Radix and Rehmannia Radix Praeparata by HPLC-UV-DPPH method / 中草药

Objective To develop an HPLC-UV-DPPH method to compare anti-oxidants of Rehmanniae Radix and Rehmanniae Radix Praeparata sample from different manufactories and to provide an effective method for the processing and quality control of traditional Chinese medicine. Methods HPLC in HPLC-UV-DPPH system was performed on Aglient Extend C18 (250 mm × 4.6 mm, 5 μm) column with gradient elution of acetonitrile-0.1% acetic acid at the flow rate of 1.0 mL/min, and the detection wavelength was at 334 nm. The column temperature was 30 ℃. Flow rate of DPPH solution is 0.5 mL/min, and detection wavelength was set at 517 nm. The total activities of the samples and the contribution rate of each component to the total activity were evaluated by the “quantity-effect” research idea, and verbascoside was regarded as a positive reference. The main anti-oxidants in original and processed herbs were identified by HPLC-FT-MS and were compared. Results The detection of HPLC-UV-DPPH method showed that there were nine anti-oxidants in Rehmanniae Radix extract, while 13 anti-oxidants were found in Rehmanniae Radix Praeparata. There were eight common anti-oxidants in the two herbs. The anti-oxidants were obviously different before and after Rehmanniae Radix processed. The activities of the antioxidants in different samples were markedly different. Anti-oxidants with higher contributions were mussaenosidic acid, echinacoside, jionoside A1/A2, verbascoside, and isoverbascoside, respectively. Conclusion The HPLC-UV-DPPH method is stable, sensitive, reproducible, and suitable for rapid screening of anti-oxidants and quality evaluation of Rehmanniae Radix and Rehmannia Radix Praeparata.

Study on chemical constituents of “decocted first and defoamed” of Ephedra Herba by UPLC-DAD-TOF/MS and HPLC-UV / 中草药

Objective To establish a method for detecting the chemical compositions of “decocted first and defoamed” of Ephedra Herba by UPLC-DAD-TOF/MS coupled with HPLC-UV, so as to clarify the difference of chemical constituents among them. Methods The analysis was performed on an ACQUITY UPLC® BEH C18 column (50 mm × 2.1 mm, 1.7 μm ) by UPLC-DAD-TOF/MS with gradient elution. The mobile phase consists of methanol and 0.1% formic acid-water at a flow rate of 0.3 mL/min. The column temperature was 40 ℃. The information of compounds was acquired on positive and negative mode. Similarly, HPLC-UV was applied for measuring the content of alkaloids respectively. The C18 column was used, the mobile phase was acetonitrile-0.1% phosphoric acid (containing 0.05% triethylamine) (99 : 1) at the flow rate of 1 mL/min, the detective wavelength was set up at 210 nm, and the column temperature was 30 ℃. Results There were less content in the upper foam, and the chemical components in the lower liquid and the whole liquid were basically same. Five alkaloids and one carboxylic acid (4-hydroxy-7-methoxyl-2-quinoline carboxylic acid) was identified from all kinds of liquids. However, the content of alkaloids in the upper foam was very low, and the content of three alkaloids in the whole solution was slightly higher than that in the lower liquid. Conclusion The defoamed method may not be related to the chemical compositions of alkaloids, but it still needs further research and verification.

Quality comparison study between wild and cultivated Astragali Radix based on absolute growth years / 中草药

Objective To compare the chemical composition and the pharmaceutical effect of anti-heart failure of wild commodity Astragali Radix (WAR) and cultivated Astragali Radix (CAR). Methods The contents of flavonoids and saponins in Astragali Radix samples were determined by HPLC-UV-ELSD. The intervention effects of wild commodity and cultivated Astragali Radix on traditional efficacy index and metabolomics were compared in rat model with heart failure induced by adriamycin. Results The contents of total flavonoids, saponin I, and saponin III in WAR were significantly higher than those in CAR, but the content of total saponins was the equivalent. Pharmacodynamics experimental results showed that both WAR and CAR could improve the general situation in rats, histopathology, cardiac function parameters, serum biochemical indicators, and BNP. However, compared with the model group, the intervention effects of the WAR on cardiac function parameters (EF, FS, and LVIDs), biochemical markers (CK) and serum BNP content were superior to the CAR, and showed significant differences. The principal component analysis showed that the metabolic profiles of the normal control group and the model group were clearly distinguished. A total of 14 potential biomarkers associated with heart failure were identified, which could be adjusted to varying degrees in WAR and CAR, of which 2-hydroxyisobutyric acid, acetone, pyruvate, and formate were significantly changed in the WAR group. Conclusion In this study, the intervention of WAR in heart failure rats was significantly better than that of CAR, which provided a scientific basis for the establishment of specification grading, the clinical rational drugs use, and the classification of Astragali Radix by pharmaceutical companies for Astragali Radix.

Pharmacokinetic study of cholesteryl-phosphoryl zidovudine in rats / 国际药学研究杂志

Objective: To develop and validate methods for determination of cholesteryl-phosphoryl zidovudine(CPZ)and its metabolite zidovudine(AZT)in rat plasma and tissues,and use the methods to investigate the pharmacokinetics of CPZ in rats. Meth- ods: An HPLC-UV method was applied for the determination of CPZ in biological samples. The biological samples were precipitated with acetonitrile at first,and then CPZ was separated on a Diamonsil C 18 column(200 mm×4.6 mm I.D.,5 μm)with a gradient elution system comprising 90% methanol and 10% isopropanol(containing 2 mmol/L cetyl trimethylammonium bromide,2% acetic acid and 0.1% ammonium hydroxide). The eluent was monitored at 266 nm by UV detector. The determination of AZT in biological samples was performed by LC-MS/MS after it was extracted from the biological samples by liquid-liquid extraction with methyl tertbutyl ether. Chro- matographic separation was performed on a Poroshell 120 EC-C 18 column(50 mm×2.1 mm I.D.,2.7 μm). Using the mobile phase con- sisted of 35% methanol and 65% water containing 0.2% acetic acid,the column was eluted by an isocratic elution with the flow rate of 0.3 ml/min. Detection of AZT and the internal standard(IS)acetaminophen was achieved by ESI MS/MS in the positive ion mode using m/z 268.2→m/z 127.0 and m/z 152.1→m/z 110.0 transitions,respectively. Results: The linear ranges for the quantitative determina- tion of CPZ and AZT were 5-400 μg/ml and 2-500 ng/ml,respectively,when 50 μl plasma was analyzed. The lower limit for the quan- tification of CPZ and AZT was 5 μg/ml and 2 ng/ml,respectively. The inter-and intra-day precision values were below 15%,and the accuracy(relative error)was within ± 13.8% in all quality control samples. CPZ was quickly metabolized in rats,while AZT was oppo-site. The half-life of AZT was about 8 h. The distribution of CPZ and AZT was more in the liver,spleen and lungs of rats,and less in the heart and kidney. Conclusion: The methods completely meet the requirements for pharmacokinetic study of CPZ in rats. The phar- macokinetic results show that CPZ could release AZT targeting liver,spleen,and lungs in rats.