Aim In the present study a RP-HPLC method was developed and validated toinvestigate the stability of baicalin aqueous solution. Methods The influences of temperature and pHon the stability of baicalin aqueous solution...Aim In the present study a RP-HPLC method was developed and validated toinvestigate the stability of baicalin aqueous solution. Methods The influences of temperature and pHon the stability of baicalin aqueous solution were investigated by classic homoiothermicacceleration test, and the pH for the most stable solution was determined. Results The time whenbaicalin suffered 10% loss was found to be 18.1 h, and the degradation activation energy of baicalinwas 79.1 kJ·moL^(-1) . The pH at which baicalin is most stable is 4.28. Conclusion The temperatureshould be kept at a lower level and the pH should be adjusted to near that for the most stablesolution in the production of baicalin preparations.展开更多
It was concluded that the described HPLC method could be used for the assayof salmon calcitonin in injection, as it offers qualified selectivity, accuracy and precision ofanalysis.
Aim A liquid chromatographic method for the determination ofcandicidin/FR-008 and related components in fermentation broth has been developed. Methods Therewere four major components in the candicidin/FR-008 complex, ...Aim A liquid chromatographic method for the determination ofcandicidin/FR-008 and related components in fermentation broth has been developed. Methods Therewere four major components in the candicidin/FR-008 complex, which were separated by HPLC under thefollowing conditions: SB-C8 column (4.6 mm x 250 mm, 5 μm) was used, the mobile phase consisted ofacetonitrileam-monium acteate (20 mmol·L^(-1) , pH 4.0) (40:60, V/V) , with a flow rate of 1 .0mL·min^(-1) , the UV detection wavelength was 380 nm, and the whole process was performed at 25℃ .Results The linearity was obtained in the range of 6.25 - 500 μg· mL^(-1) candicidin/FR-008 withthe regression equation of Y = 20 461 x + 30 748 and the correlation coefficient of 0.999 1. Theinstrument precision was 1.84% and the method precision was 3.8%. Conclusion This method isaccurate, rapid and simple; it can be used for determination of candicidin/FR-008 and relatedcomponents in fermentation broth.展开更多
Fucoxanthin content of five brown seaweed species of East Java collected from Talango district (Madura sea-Jawa sea) namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargas...Fucoxanthin content of five brown seaweed species of East Java collected from Talango district (Madura sea-Jawa sea) namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargassum echinocarpum were determined and samples were collected using Global Positioning System (GPS). Fucoxanthin from those samples was determined using Thin Layer Chromatography (TLC), High Pressure Liquid Chromatography (HPLC) and Spectrophotometer UV-Vis and the results were then calculated using Seely equation. The pigments separation using HPLC gave a better result compared to TLC, and beside fucoxanthin otlher pigments namely chlorophyll and β carotene were also identified in these samples. Four points of sampling location were chosen using GPS and spot with coordinate positions observed were 113.94444° EL-7.08795° SA; 113.94231° EL-7.08913° SA. The results showed that fucoxanthin content were as follow: Padina australis 0.2674± 0.0046 mg/g; Turbinaria conoides 0.2134± 0.0100 mg/g; Sargassum filipendula 0.1957 ± 0.0173 mg/g; Sargassum cinereum 0.1640 ± 0.0092 mg/g and Sargassum echinocarpum 0.1576 ± 0.0001 mg/g. It can be concluded that Padina australis and Turbinaria conoides contain the most amount of fucoxanthin and it is possible to be cultivated as edible brown seaweed fucoxanthin resources.展开更多
The persistence of malachite green (MG), and its metabolite leucomalachite green (LMG), in fish tissues is still unclear, leading to many trade disputes. In this research, we established and evaluated an HPLC method t...The persistence of malachite green (MG), and its metabolite leucomalachite green (LMG), in fish tissues is still unclear, leading to many trade disputes. In this research, we established and evaluated an HPLC method that could detect MG and LMG simultaneously, and then investigated the persistence of these two toxins in the tissues of juvenile perch (Lateolabrax japonicus) post sub-chronic MG exposure at 1.0 mg/L. Exposure lasted for 2 h everyday and was repeated six times. The perch were then placed in MG-free seawater for 100 d to eliminate the toxins. Results show that MG accumulated in the tissues, including the gills, liver, muscle, blood and viscera, and then was metabolized rapidly to LMG. The concentrations of these two toxins increased significantly with the accumulation process. In general, the highest concentrations of MG and LMG in all tissue exceeded 1 000 μg/kg, except for MG in the muscle. The order of accumulation levels (highest to lowest) of MG was gill>blood>liver>viscera>muscle, while that of LMG was liver>blood>gill>viscera>muscle. High levels of MG or LMG could persist for several hours but decreased rapidly during the elimination process. The concentration of LMG was much higher than that of MG during the experiment, especially in the gill, liver and blood. Therefore, the three tissues play important roles in toxin accumulation, biotransformation, and elimination. Although the MG and LMG concentrations in muscle were much lower than in other tissues, the content still exceeded the European minimum required performance limit (MRPL), even after 2 400 h (100 d) of elimination. This demonstrates that it is extremely difficult to eliminate MG and LMG from tissues of perch, and therefore use of these toxins is of concern to public health.展开更多
Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain mult...Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas.展开更多
Three kinds of polysaccharides: GFW, GFH and GFA, were sequentially extracted from a red alga Gloiopeltisfurcata with 25℃ and 85℃ water, and 60℃ 4% NaOH water solution. Based on the defatted alga, the yields of th...Three kinds of polysaccharides: GFW, GFH and GFA, were sequentially extracted from a red alga Gloiopeltisfurcata with 25℃ and 85℃ water, and 60℃ 4% NaOH water solution. Based on the defatted alga, the yields of the polysaccharide were 57.9%, 2.5% and 2.6%, respectively. Their monosaccharide compositions, average molecular weights and structural characters were determined by gas chromatography (GC), high performance liquid chromatography (HPLC), fourier transform infrared spectroscopy (FTIR) or ^13C-NMR spectroscopy. The results showed that GFW, GFH and GFA were all composed of D-galactose (Gal) and 3,6-anhydro-L-galactose (AnG), and particularly GFA also contained xylose (Xyl). The average molecular weights of GFW, GFH and GFA were 22.6 kD, 26.5 kD and 49.8 kD, respectively, with the respective sulfate content 31.2%, 25.1% and 22.7%. The data of FTIR and ^13C-NMR confirmed the sulfate ester location at C6 ofgalactose. It is concluded that all the three polysaecharides extracted from Gloiopeltisfurcata were sulfated galactans, two being sulfated-agarose, and one being xylose-containing sulfated galactan.展开更多
To study the effect of cultivation system (conventional and organic) on potato tuber components, 42 parameters (anti-nutritives, micro- and macro-elements and 23 metabolites) were studied in three multi-resistant ...To study the effect of cultivation system (conventional and organic) on potato tuber components, 42 parameters (anti-nutritives, micro- and macro-elements and 23 metabolites) were studied in three multi-resistant Hungarian potato varieties for three years in 2007-2009. Discriminant analysis of data proved that all investigated factors (farming technology, genotype and season/year) had significant effect on metabolites. Reversed phase high performance liquid chromatographic (HPLC-DAD, HPLC-MS) and elemental analysis methods have been adapted to quantify the major components, i.e., steroidal alkaloids, nitrite, nitrate, sugars, amino acids and micro-elements, in potato tubers. The absolute amount and changes of tuber components were influenced differentially by the technology, genotype and season in a complex manner. Any examined component, except nitrate content, was found to be significantly higher or lower consistently in relation to the production practice (organic or conventional) during the three years trials. Under the examined circumstances, no consequent positive effect of organic fanning on the total amount of anti-nutritive components, vitamins or micro- and macro-elements of potato tubers could be proven.展开更多
Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmemb...Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmembrane pressure, temperature and axial flow-rate on the membrane fluxes were analyzed, and then the SP of the ultrafiltrate after follow-up resin adsorption by HPLC was investigated. The results in- dicated that US could significantly enhance the membrane fluxes. The optimal con- ditions obtained was as follows: 0.60 W/cm2 US power, axial flow-rate of 80 L/h, operation temperature 30 ~C, transmembrane pressure 0.10 MPa. US increased the absorption capacity of the absorbent resin during the following stage. The HPLC analysis also showed that catechins were purified to some extent as the ultrafiltrate was treated by US and macroporous resin, indicating the technology of US en- hancement coupled with UF showed the potential for concentration and purification of SP by absorbent resins.展开更多
Biological treatment efficiency of six pharmaceutical compounds (acetazolamide, metronidazole, opipramol, piracetam, salicylamide and tinidazole) was evaluated using lab-scale Sequencing Batch Reactor (SBR). Compa...Biological treatment efficiency of six pharmaceutical compounds (acetazolamide, metronidazole, opipramol, piracetam, salicylamide and tinidazole) was evaluated using lab-scale Sequencing Batch Reactor (SBR). Comparative biological degradation processes of two types of activated sludge from municipal and pharmaceutical industry sewage treatment plants were examined. Three different organic loadings (0.05 g COD/g MLSS.d, 0.1 g COD/g MLSS.d and 0.2 g COD/g MLSS-d) and reaction time on the efficiency of Active Pharmaceutical Ingredient (API) decomposition were examined. Chemical oxygen demand, non-purgeable organic carbon as well as ammonium nitrogen contents were monitored by standard methods. Percentage of API decomposition was analysed by High Performance Liquid Chromatography (HPLC). The overall API removal efficiency was strictly dependent on the type of activated sludge origin. The main biodegradation products were identified using HPLC-MS,1H NMR and 13C NMR methods as e.g. ({4-[3-(5H-dibenzo[b,f]azepin-5-yl]piperazin-l-yl}methanamine) and (2-amino-1,3,4-thiadiazol-5-sulfonamide) for opipramol and acetazolamide respectively.展开更多
Aflatoxins are produced mainly by Aspergillus flavus and Aspergillus parasiticus, and can be found in many grains such as peanuts, soybeans and com. This study aimed to qualitatively and quantitatively evaluate the pr...Aflatoxins are produced mainly by Aspergillus flavus and Aspergillus parasiticus, and can be found in many grains such as peanuts, soybeans and com. This study aimed to qualitatively and quantitatively evaluate the production of aflatoxin in liquid media using strains of Aspergillus flavus obtained from peanuts marketed in the city of Fortaleza, CEo Strains of Aspergillus flavus were inoculated into a liquid medium malt extract and after 2 days inoculated into a second medium containing sucrose 5%, MgSO4·7H20 0.1%, KH2PO4 1%, ZnSO4·7H2O 0.0176 g, and cultured for 3 more days. The media were kept at room temperature ranging from 24°C to 32 °C with agitation of 130 rpm and aeration of 4.17 Llmin. Qualitative analysis was performed by thin layer chromatography and quantitatively by high performance liquid chromatography with fluorescence detection, demonstrating the production of aflatoxin B I (588 mg/L) and B2 (929 mg/L).展开更多
The study examined the photodegradative efficiency of ZnO and TiO2 in degradation of antibiotics in aqueous matrices. Among several types of antibiotics, four antibiotics were chosen to feature the major classes of th...The study examined the photodegradative efficiency of ZnO and TiO2 in degradation of antibiotics in aqueous matrices. Among several types of antibiotics, four antibiotics were chosen to feature the major classes of these compounds: amoxicillin, erythromycin, streptomycin and ciprofloxacin. Degradation of antibiotic solutions was carried out mainly under UV-light irradiation in a set time with the presence of small quantity of zinc oxide or titanium dioxide. Solutions were analyzed with HPLC chromatography and degradation percentages were calculated from ratio between pick area associated to no degraded drug solution and degraded drug solution's pick area. Meanwhile, toxicity of antibiotics and degrading compounds were investigated using a biosensor system, consisting of Clark's electrode associated with a portion of agar medium culture containing Saccharomyces Cerevisiae yeast cells. This way, it was possible to define the oxygen that was consumed by yeast cells. Toxicity associated to antibiotics and degrading products are related to decrease of oxygen concentration in solution. It is clear that zinc oxide is slower than titanium dioxide to degrade antibiotics, but zinc oxide shows better photodegradation efficiency than titanium dioxide in spite of its small specific superficial area.展开更多
We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column usin...We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid (TFA) aqueous solution (A) and methanol (B). The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL (r2= 0.9998), 9.38-1407 μg/mL (rz = 0.9999), 80.6-8060μg/mL (r2 = 0.9999) and 2.10---630μg/mL (r2 = 0.9987) with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.展开更多
In the present study, we developed a sensitive and efficient high performance liquid chromatography (HPLC) method for the simultaneous determination of three ginsenosides (Rg1, Re, Rb1) in rat plasma. Chromatograp...In the present study, we developed a sensitive and efficient high performance liquid chromatography (HPLC) method for the simultaneous determination of three ginsenosides (Rg1, Re, Rb1) in rat plasma. Chromatographic separation was performed on a C18 (150 min×4.6 mm) column utilizing gradient elution profile and a mobile phase consisting of (A) water and (B) acetonitrile. The calibration curve, with a great correlation coefficient greater than 0.998, was linear over the range of 1.0-30.0 μg/mL for ginsenoside Rgl, 0.5-15.0 μg/mL for ginsenoside Re, and 0.5-200.0 μg/mL for ginsenoside Rb1. The intra- and inter-day precisions for three ginsenosides (Rg1, Re, Rb1) were all less than 6.0%, and average recovery, examined at three concentration levels, ranged from 96.1% to 118.6%. The samples was stable within 24 h at 4 ℃ storage, and 30 d at -20 ℃ storage with three freeze-thaw-assay cycles. The low limits of quantification (LOQ) were 1.0, 0.5 and 0.5 μg/mL for Rg1, Re and Rb1, respectively. Taken together, the newly developed method was successfully applied to study the pharmacokinetics of ginsenoside Rg1, Re and Rb1 in rat plasma after intravenous administration of SHENMAI injection (SMI).展开更多
A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal st...A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal standard l-(3-((6,7-bis(2- methoxyethoxy)quinazolin-4-yl)amino)phenyl)ethanone were extracted from mice plasma samples using liquid-liquid extraction with a mixed solvent of methyl t-butyl ether and ethyl acetate(9:1,v/v).Chromatographic separation was performed on a Luna C|_(18)column(4.6 mm×250 mm,5μm)with acetonitrile:5 mM potassium phosphate buffer pH=5.2(41:59,v/v)as the mobile phase.UV detector was set at the wavelength of 345 nm,and the flow rate was 1.0 mL/min.The calibration curve was linear over the range of 20-10 000 ng/mL with acceptable intra-and inter-day precision and accuracy.The intra-day and inter-day precisions were within the range of 1.69%—5.66%,and the accuracies of intra-and inter-day assays were within the range of 105%—113%. The mean recoveries were 85.2%and 96.1%for erlotinib and IS,respectively.This method was successfully applied to a pharmacokinetic study in tumor bearing BALB/c nude mice following single oral administration at the dose of 12.5 mg/kg. The main pharmacokinetic parameters were as follows:C_(max)was 4.67μg/mL,T_(max)was 1.0 h,T_(1/2)was 2.78 h,and AUC_(0-24h)was 18.0μg/mL·h.展开更多
A simple method based on hollow fiber liquid-phase microextraction (HF-LPME) followed by high performance liquid chro-matography (HPLC) analysis was successfully developed for the determination of UV filters in cosmet...A simple method based on hollow fiber liquid-phase microextraction (HF-LPME) followed by high performance liquid chro-matography (HPLC) analysis was successfully developed for the determination of UV filters in cosmetic products. A canular extractor was assembled by mounting a hollow fiber inside an external tube with a tee-connector. The organic solvent was immobilized into the fiber to form a liquid membrane as the acceptor phase. The sample was continuously injected into the extractor and the UV filters were extracted from the aqueous sample into organic acceptor phase. The main parameters affecting HF-LPME including extraction solvent, sample volume, sample flow rate, pH values and ionic strength were investigated. Toluene has been verified to be suitable as the acceptor phase. Under the optimized HF-LPME conditions, the enrichment factors of five UV filters varying from 24 to 57 were achieved. The limits of detection for the five UV filters were in the range of 1-100 μg L-1 .The relative standard deviations (RSDs) of HF-LPME and HPLC analysis were lower than 5.2%. The proposed method has been successfully applied to the analysis of the varied cosmetic products.展开更多
文摘Aim In the present study a RP-HPLC method was developed and validated toinvestigate the stability of baicalin aqueous solution. Methods The influences of temperature and pHon the stability of baicalin aqueous solution were investigated by classic homoiothermicacceleration test, and the pH for the most stable solution was determined. Results The time whenbaicalin suffered 10% loss was found to be 18.1 h, and the degradation activation energy of baicalinwas 79.1 kJ·moL^(-1) . The pH at which baicalin is most stable is 4.28. Conclusion The temperatureshould be kept at a lower level and the pH should be adjusted to near that for the most stablesolution in the production of baicalin preparations.
文摘It was concluded that the described HPLC method could be used for the assayof salmon calcitonin in injection, as it offers qualified selectivity, accuracy and precision ofanalysis.
文摘Aim A liquid chromatographic method for the determination ofcandicidin/FR-008 and related components in fermentation broth has been developed. Methods Therewere four major components in the candicidin/FR-008 complex, which were separated by HPLC under thefollowing conditions: SB-C8 column (4.6 mm x 250 mm, 5 μm) was used, the mobile phase consisted ofacetonitrileam-monium acteate (20 mmol·L^(-1) , pH 4.0) (40:60, V/V) , with a flow rate of 1 .0mL·min^(-1) , the UV detection wavelength was 380 nm, and the whole process was performed at 25℃ .Results The linearity was obtained in the range of 6.25 - 500 μg· mL^(-1) candicidin/FR-008 withthe regression equation of Y = 20 461 x + 30 748 and the correlation coefficient of 0.999 1. Theinstrument precision was 1.84% and the method precision was 3.8%. Conclusion This method isaccurate, rapid and simple; it can be used for determination of candicidin/FR-008 and relatedcomponents in fermentation broth.
文摘Fucoxanthin content of five brown seaweed species of East Java collected from Talango district (Madura sea-Jawa sea) namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargassum echinocarpum were determined and samples were collected using Global Positioning System (GPS). Fucoxanthin from those samples was determined using Thin Layer Chromatography (TLC), High Pressure Liquid Chromatography (HPLC) and Spectrophotometer UV-Vis and the results were then calculated using Seely equation. The pigments separation using HPLC gave a better result compared to TLC, and beside fucoxanthin otlher pigments namely chlorophyll and β carotene were also identified in these samples. Four points of sampling location were chosen using GPS and spot with coordinate positions observed were 113.94444° EL-7.08795° SA; 113.94231° EL-7.08913° SA. The results showed that fucoxanthin content were as follow: Padina australis 0.2674± 0.0046 mg/g; Turbinaria conoides 0.2134± 0.0100 mg/g; Sargassum filipendula 0.1957 ± 0.0173 mg/g; Sargassum cinereum 0.1640 ± 0.0092 mg/g and Sargassum echinocarpum 0.1576 ± 0.0001 mg/g. It can be concluded that Padina australis and Turbinaria conoides contain the most amount of fucoxanthin and it is possible to be cultivated as edible brown seaweed fucoxanthin resources.
基金Supported by the Special Fund of Chinese Government for Basic Scientific Research Operations in Commonweal Research Institute (Yellow Sea Fisheries Research Institute) (No. 2007-qn-12)the Strategic Research Grant of the Databases and Risk Analysis of POPs in Aquatic Products (No. 2005DIB4J049)the Standard System Research on Quality and Safety of Aquatic Products (No. 2004DEA70880)
文摘The persistence of malachite green (MG), and its metabolite leucomalachite green (LMG), in fish tissues is still unclear, leading to many trade disputes. In this research, we established and evaluated an HPLC method that could detect MG and LMG simultaneously, and then investigated the persistence of these two toxins in the tissues of juvenile perch (Lateolabrax japonicus) post sub-chronic MG exposure at 1.0 mg/L. Exposure lasted for 2 h everyday and was repeated six times. The perch were then placed in MG-free seawater for 100 d to eliminate the toxins. Results show that MG accumulated in the tissues, including the gills, liver, muscle, blood and viscera, and then was metabolized rapidly to LMG. The concentrations of these two toxins increased significantly with the accumulation process. In general, the highest concentrations of MG and LMG in all tissue exceeded 1 000 μg/kg, except for MG in the muscle. The order of accumulation levels (highest to lowest) of MG was gill>blood>liver>viscera>muscle, while that of LMG was liver>blood>gill>viscera>muscle. High levels of MG or LMG could persist for several hours but decreased rapidly during the elimination process. The concentration of LMG was much higher than that of MG during the experiment, especially in the gill, liver and blood. Therefore, the three tissues play important roles in toxin accumulation, biotransformation, and elimination. Although the MG and LMG concentrations in muscle were much lower than in other tissues, the content still exceeded the European minimum required performance limit (MRPL), even after 2 400 h (100 d) of elimination. This demonstrates that it is extremely difficult to eliminate MG and LMG from tissues of perch, and therefore use of these toxins is of concern to public health.
基金partly supported by "Accordo di Programma, affermazione in Edolo del Centro di Eccellenza Università della Montagna" MIURUniversità degli Studi di Milano, prot. no. 386 1293-05/08/2011 and by Fondazione della Comunità Bresciana- Onlus
文摘Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas.
基金supported in part by the International Science and Technology Cooperation Program of China(2007DFA30980)the National High Technology Research and Development Program(2007AA09Z445)the National Natural Science Foundation of China(30870506)
文摘Three kinds of polysaccharides: GFW, GFH and GFA, were sequentially extracted from a red alga Gloiopeltisfurcata with 25℃ and 85℃ water, and 60℃ 4% NaOH water solution. Based on the defatted alga, the yields of the polysaccharide were 57.9%, 2.5% and 2.6%, respectively. Their monosaccharide compositions, average molecular weights and structural characters were determined by gas chromatography (GC), high performance liquid chromatography (HPLC), fourier transform infrared spectroscopy (FTIR) or ^13C-NMR spectroscopy. The results showed that GFW, GFH and GFA were all composed of D-galactose (Gal) and 3,6-anhydro-L-galactose (AnG), and particularly GFA also contained xylose (Xyl). The average molecular weights of GFW, GFH and GFA were 22.6 kD, 26.5 kD and 49.8 kD, respectively, with the respective sulfate content 31.2%, 25.1% and 22.7%. The data of FTIR and ^13C-NMR confirmed the sulfate ester location at C6 ofgalactose. It is concluded that all the three polysaecharides extracted from Gloiopeltisfurcata were sulfated galactans, two being sulfated-agarose, and one being xylose-containing sulfated galactan.
文摘To study the effect of cultivation system (conventional and organic) on potato tuber components, 42 parameters (anti-nutritives, micro- and macro-elements and 23 metabolites) were studied in three multi-resistant Hungarian potato varieties for three years in 2007-2009. Discriminant analysis of data proved that all investigated factors (farming technology, genotype and season/year) had significant effect on metabolites. Reversed phase high performance liquid chromatographic (HPLC-DAD, HPLC-MS) and elemental analysis methods have been adapted to quantify the major components, i.e., steroidal alkaloids, nitrite, nitrate, sugars, amino acids and micro-elements, in potato tubers. The absolute amount and changes of tuber components were influenced differentially by the technology, genotype and season in a complex manner. Any examined component, except nitrate content, was found to be significantly higher or lower consistently in relation to the production practice (organic or conventional) during the three years trials. Under the examined circumstances, no consequent positive effect of organic fanning on the total amount of anti-nutritive components, vitamins or micro- and macro-elements of potato tubers could be proven.
基金Supported by Special Fund for Agro-scientific Research in the Public Interest(201303080)Hubei Agricultural Science&Technology Innovation Center Project(2014-620-007-001)Natural Science Foundation of Hubei Province of China(2013CFB053)
文摘Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmembrane pressure, temperature and axial flow-rate on the membrane fluxes were analyzed, and then the SP of the ultrafiltrate after follow-up resin adsorption by HPLC was investigated. The results in- dicated that US could significantly enhance the membrane fluxes. The optimal con- ditions obtained was as follows: 0.60 W/cm2 US power, axial flow-rate of 80 L/h, operation temperature 30 ~C, transmembrane pressure 0.10 MPa. US increased the absorption capacity of the absorbent resin during the following stage. The HPLC analysis also showed that catechins were purified to some extent as the ultrafiltrate was treated by US and macroporous resin, indicating the technology of US en- hancement coupled with UF showed the potential for concentration and purification of SP by absorbent resins.
文摘Biological treatment efficiency of six pharmaceutical compounds (acetazolamide, metronidazole, opipramol, piracetam, salicylamide and tinidazole) was evaluated using lab-scale Sequencing Batch Reactor (SBR). Comparative biological degradation processes of two types of activated sludge from municipal and pharmaceutical industry sewage treatment plants were examined. Three different organic loadings (0.05 g COD/g MLSS.d, 0.1 g COD/g MLSS.d and 0.2 g COD/g MLSS-d) and reaction time on the efficiency of Active Pharmaceutical Ingredient (API) decomposition were examined. Chemical oxygen demand, non-purgeable organic carbon as well as ammonium nitrogen contents were monitored by standard methods. Percentage of API decomposition was analysed by High Performance Liquid Chromatography (HPLC). The overall API removal efficiency was strictly dependent on the type of activated sludge origin. The main biodegradation products were identified using HPLC-MS,1H NMR and 13C NMR methods as e.g. ({4-[3-(5H-dibenzo[b,f]azepin-5-yl]piperazin-l-yl}methanamine) and (2-amino-1,3,4-thiadiazol-5-sulfonamide) for opipramol and acetazolamide respectively.
文摘Aflatoxins are produced mainly by Aspergillus flavus and Aspergillus parasiticus, and can be found in many grains such as peanuts, soybeans and com. This study aimed to qualitatively and quantitatively evaluate the production of aflatoxin in liquid media using strains of Aspergillus flavus obtained from peanuts marketed in the city of Fortaleza, CEo Strains of Aspergillus flavus were inoculated into a liquid medium malt extract and after 2 days inoculated into a second medium containing sucrose 5%, MgSO4·7H20 0.1%, KH2PO4 1%, ZnSO4·7H2O 0.0176 g, and cultured for 3 more days. The media were kept at room temperature ranging from 24°C to 32 °C with agitation of 130 rpm and aeration of 4.17 Llmin. Qualitative analysis was performed by thin layer chromatography and quantitatively by high performance liquid chromatography with fluorescence detection, demonstrating the production of aflatoxin B I (588 mg/L) and B2 (929 mg/L).
文摘The study examined the photodegradative efficiency of ZnO and TiO2 in degradation of antibiotics in aqueous matrices. Among several types of antibiotics, four antibiotics were chosen to feature the major classes of these compounds: amoxicillin, erythromycin, streptomycin and ciprofloxacin. Degradation of antibiotic solutions was carried out mainly under UV-light irradiation in a set time with the presence of small quantity of zinc oxide or titanium dioxide. Solutions were analyzed with HPLC chromatography and degradation percentages were calculated from ratio between pick area associated to no degraded drug solution and degraded drug solution's pick area. Meanwhile, toxicity of antibiotics and degrading compounds were investigated using a biosensor system, consisting of Clark's electrode associated with a portion of agar medium culture containing Saccharomyces Cerevisiae yeast cells. This way, it was possible to define the oxygen that was consumed by yeast cells. Toxicity associated to antibiotics and degrading products are related to decrease of oxygen concentration in solution. It is clear that zinc oxide is slower than titanium dioxide to degrade antibiotics, but zinc oxide shows better photodegradation efficiency than titanium dioxide in spite of its small specific superficial area.
基金Program for Changjiang Scholar and Innovative Team in University(Grant No.985-2-063-112)
文摘We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid (TFA) aqueous solution (A) and methanol (B). The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL (r2= 0.9998), 9.38-1407 μg/mL (rz = 0.9999), 80.6-8060μg/mL (r2 = 0.9999) and 2.10---630μg/mL (r2 = 0.9987) with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.
基金Science and Technology Research project of Heilongjiang Province Department of Education(Grant No.12541740)
文摘In the present study, we developed a sensitive and efficient high performance liquid chromatography (HPLC) method for the simultaneous determination of three ginsenosides (Rg1, Re, Rb1) in rat plasma. Chromatographic separation was performed on a C18 (150 min×4.6 mm) column utilizing gradient elution profile and a mobile phase consisting of (A) water and (B) acetonitrile. The calibration curve, with a great correlation coefficient greater than 0.998, was linear over the range of 1.0-30.0 μg/mL for ginsenoside Rgl, 0.5-15.0 μg/mL for ginsenoside Re, and 0.5-200.0 μg/mL for ginsenoside Rb1. The intra- and inter-day precisions for three ginsenosides (Rg1, Re, Rb1) were all less than 6.0%, and average recovery, examined at three concentration levels, ranged from 96.1% to 118.6%. The samples was stable within 24 h at 4 ℃ storage, and 30 d at -20 ℃ storage with three freeze-thaw-assay cycles. The low limits of quantification (LOQ) were 1.0, 0.5 and 0.5 μg/mL for Rg1, Re and Rb1, respectively. Taken together, the newly developed method was successfully applied to study the pharmacokinetics of ginsenoside Rg1, Re and Rb1 in rat plasma after intravenous administration of SHENMAI injection (SMI).
基金National Integrity Innovational Technology Platform of New Drug and Development(Grant No.2009ZX09301- 010).
文摘A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal standard l-(3-((6,7-bis(2- methoxyethoxy)quinazolin-4-yl)amino)phenyl)ethanone were extracted from mice plasma samples using liquid-liquid extraction with a mixed solvent of methyl t-butyl ether and ethyl acetate(9:1,v/v).Chromatographic separation was performed on a Luna C|_(18)column(4.6 mm×250 mm,5μm)with acetonitrile:5 mM potassium phosphate buffer pH=5.2(41:59,v/v)as the mobile phase.UV detector was set at the wavelength of 345 nm,and the flow rate was 1.0 mL/min.The calibration curve was linear over the range of 20-10 000 ng/mL with acceptable intra-and inter-day precision and accuracy.The intra-day and inter-day precisions were within the range of 1.69%—5.66%,and the accuracies of intra-and inter-day assays were within the range of 105%—113%. The mean recoveries were 85.2%and 96.1%for erlotinib and IS,respectively.This method was successfully applied to a pharmacokinetic study in tumor bearing BALB/c nude mice following single oral administration at the dose of 12.5 mg/kg. The main pharmacokinetic parameters were as follows:C_(max)was 4.67μg/mL,T_(max)was 1.0 h,T_(1/2)was 2.78 h,and AUC_(0-24h)was 18.0μg/mL·h.
基金supported by the National Natural Science Foundation of China (90813015 & 20935002)
文摘A simple method based on hollow fiber liquid-phase microextraction (HF-LPME) followed by high performance liquid chro-matography (HPLC) analysis was successfully developed for the determination of UV filters in cosmetic products. A canular extractor was assembled by mounting a hollow fiber inside an external tube with a tee-connector. The organic solvent was immobilized into the fiber to form a liquid membrane as the acceptor phase. The sample was continuously injected into the extractor and the UV filters were extracted from the aqueous sample into organic acceptor phase. The main parameters affecting HF-LPME including extraction solvent, sample volume, sample flow rate, pH values and ionic strength were investigated. Toluene has been verified to be suitable as the acceptor phase. Under the optimized HF-LPME conditions, the enrichment factors of five UV filters varying from 24 to 57 were achieved. The limits of detection for the five UV filters were in the range of 1-100 μg L-1 .The relative standard deviations (RSDs) of HF-LPME and HPLC analysis were lower than 5.2%. The proposed method has been successfully applied to the analysis of the varied cosmetic products.