The chemical components of the essential oils in the barks and leaves of Eucommia ulmoides Oliver were analyzed and compared by chromatograms and mass spectra technique, heuristic evolving latent projections (HELP), a...The chemical components of the essential oils in the barks and leaves of Eucommia ulmoides Oliver were analyzed and compared by chromatograms and mass spectra technique, heuristic evolving latent projections (HELP), alternative moving window factor analysis (AMWFA) algorithms and normalization method based on the peak areas; the flavones in the barks and leaves of Eucommia ulmoides Oliver were separated on an ODS column by gradient elution carried out with the flow phase consisting of water, methanol and phosphoric acid (0.1%), and their contents were quantitatively determined by standard curve method and diode array detection (DAD) at 362 nm. The results show that 68 and 73 compounds respectively from essential oils of the barks and leaves of Eucommia ulmoides Oliver are identified, and there are 33 mutual compounds among 108 compounds determined. The total contents of these volatile components of the two samples possess 92.9% and 97.75% of the gross of the relevant essential oils, respectively; the contents of the rutin, quercetin and kaempferol in the barks and leaves of Eucommia ulmoides Oliver are 0.016 9, 0.003 6, 0.002 1 and 0.064 4, 0.030 2, 0.010 0 mg/g, respectively, and the determination recoveries are 95.2%-106.2%. The comparative analysis shows that for the barks and leaves of Eucommia ulmoides Oliver, there are significant differences in their components of the relevant essential oils and flavones.展开更多
To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liq...To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.展开更多
This paper investigates the occurrence of sulphonamide and diaminopyrimidine antibiotics in wastewater and sludge from wastewater treatment plants. In our experiment, they were isolated from wastewater using the solid...This paper investigates the occurrence of sulphonamide and diaminopyrimidine antibiotics in wastewater and sludge from wastewater treatment plants. In our experiment, they were isolated from wastewater using the solid phase extraction method. In the case of sludge, pressurized solvent extraction techniques were used followed by solid phase extraction. The solid phase extraction method was used for purification and concentration. Sulphonamide and diaminopyrimidine antibiotics were determined using high performance liquid chromatography with diode-array detection. The selected antibiotics were determined in real sludge samples collected from the wastewater treatment plant in Brno-Mod^ice and in real wastewater samples collected from the wastewater treatment plant located on the grounds of the University of Veterinary and Pharmaceutical Sciences in Brno, using the developed and optimized method. Analyses showed that real samples of wastewater contained sulphathiazole 11.82μg/L at the inflow (7.1 μg/L at the outflow), sulphapyridine 18.57 I.tg/L (12.2 μg/L), sulphamethazine 13.52 μg/L (8.44 μg/L), sulphamethoxazole 14.06 lag/L (9.34 Ixg/L) and trimethoprim 521.4 lag/L (422.29 μg/L). Here it is demonstrated that drugs are removed through the wastewater treatment procedure only partially.展开更多
Beer can be a rich source of phenolic acids in the diet. The present review summarizes the current state of work on phenolic acids in beer presented in the cited papers. In an overview, 10 hydroxybenzoic acids, three ...Beer can be a rich source of phenolic acids in the diet. The present review summarizes the current state of work on phenolic acids in beer presented in the cited papers. In an overview, 10 hydroxybenzoic acids, three related aldehydes, two phenylacetic acids and eight hydroxycinnamic acids in beer are being reported. This review compares the phenolic acids content in alcoholic and non-alcoholic beers from Czech Republic, Germany, Italy, Austria and Poland, which had been examined by several authors. The quantification was achieved by HPLC with ultraviolet, diode array, coulometric array or fluorimetric detection. Ferulic acid is the main phenolic acid in all beers that had been studied, followed by p-coumaric, vanillic, caffeic, p-OH-benzoic and sinapic acids. Most of the phenolic acids in beer are present as bound forms and only a small portion can be detected as free compounds. The content of the phenolic acids in the non-alcoholic beers is lower than in the alcoholic beers mainly due to differences in the production process, yeast strains used, dealcoholization of beer etc..展开更多
The crosstalk caused by oblique incident ray on a PIN detector array is analyzed. An integral expression of crosstalk factor in relation to incident angle and structure parameters is deduced and the correctness of the...The crosstalk caused by oblique incident ray on a PIN detector array is analyzed. An integral expression of crosstalk factor in relation to incident angle and structure parameters is deduced and the correctness of the deduction is tested and verified.展开更多
SEM-EDS (scanning electron microscopy-energy dispersive spectrometry) and HPLC (high performance liquid chromatography) with DAD (diode array detection) were used to examine metal-wrapped coloured textiles. The ...SEM-EDS (scanning electron microscopy-energy dispersive spectrometry) and HPLC (high performance liquid chromatography) with DAD (diode array detection) were used to examine metal-wrapped coloured textiles. The sample was provided from Azerbaijan History Museum. Material included silk and thin wire. SEM micrographs showed that the metal strip had 250μm width and 6 9m thickness. SEM-EDS results indicated elemental composition of the wrapping: the presence of gold, silver as the components of the gilt metals. Furthermore, sulphur and chlorine were determined as contaminants. EDS analysis also revealed that both sides were gildered. Colouring compounds in the same sample were identified by HPLC-DAD. The major colouring compound found in the red fibre sample in large quantity was carminic acid and fuchsin components. The presence of fuchsin, which is a synthetic dye, dates the sample between the end of 19th and beginning of 20th century. Fisetin, which is a natural dye, was detected in the yellow fibre.展开更多
Petrovska klobasa is a traditional dry fermented sausage produced in the Autonomous Province of Vojvodina. Formation of nine hiogenic amines was determined in three sausage groups produced from hot deboned (A1) and ...Petrovska klobasa is a traditional dry fermented sausage produced in the Autonomous Province of Vojvodina. Formation of nine hiogenic amines was determined in three sausage groups produced from hot deboned (A1) and cold meat (B1, B3) during drying and ripening in traditional room (A1, B1) and in industrial ripening chamber (B3). Dansyl chloride derived amines were analysed by high-performance liquid chromatography with diode-array detector (HPLC-DAD) on Eclipse XDB-C18 column. Histamine, the most important amine from food safety point of view, was not found in any of the analyzed samples. Serotonin and spermidine were also not detected in any samples, while spermin was determined in all analyzed samples. At the end of drying, phenylethylamine was the predominant amine in A1 sausage group (51.6 mg/kg), and tryptamine in B1 (38.1 mg/kg) and B3 (28.7 mg/kg) sausage groups. At the end of ripening, tryptamine was the predominant biogenic amine in all sausage groups (133, 121 and 39.8 mg/kg in A1, B1 and B3 groups, respectively). Total level of biogenic amines in all investigated sausages did not exceed 174 mg/kg at the end of drying and 238 mg/kg at the end of ripening period. Tryptamine and cadaverine may be used as indicators of total biogenic amines for sausages produced in traditional and indusrial conditions from hot deboned and cold meat.展开更多
Zea mays L. is one of the biggest cropping systems among the sustainable development agronomy. Pollen from this crop source is unexplored and apiculture can be a good partner adding value to the product and creating n...Zea mays L. is one of the biggest cropping systems among the sustainable development agronomy. Pollen from this crop source is unexplored and apiculture can be a good partner adding value to the product and creating new jobs helping to solve some social issues as unemployment. However, food safety is crucial, thus the aim of this study was to explore the flavonoid/phenolic profiles from Z. mays L. pollen as a fingerprint for this plant identification and also to demonstrate how the method of bee pollen samples (honeybee collected pollen) is applied. For this purpose, several sources ofZ. mays L. pollen were analyzed, including corn hybrids and genetic modified samples collected at the breeding fields. For this work, samples were taken at several years from 2000 to 2012 and collected from different countries and locations, such as Portugal, Mexico and Brazil. Results showed, for the first time, that the fingerprint (flavonoid/phenolic profile) for Z. mays L. pollen does not change over the time of sampling neither with the region of harvesting. The high performance liquid chromatography-diode array detector (HPLC/DAD) fingerprints of phenolic/flavonoid extract from Z. mays remain unchanged for all samples analyzed from different countries, hybrids and/or genetic modified plants. This is also the first study reporting these phenolic compounds not only in pollen collected directly from hybrid plants, but also in Z. mays bee pollen. The described fingerprinting method is easy, fast and accurate for the characterization of Z. mays L. pollen samples and complete microscopic analysis because it is species-specific.展开更多
A sensitive and specific high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of metformin hydrochloride (HCI) in human plasma. The HPLC method consis...A sensitive and specific high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of metformin hydrochloride (HCI) in human plasma. The HPLC method consists of isocratic eluation with a mixture of 60% buffer (10 mM sodium dihyrogenphosphate-10 mM sodium dodecyl sulphate) and 40% acetonitrile with final pH 7.0 with flow rate of 1.0 mL/min on a Kromasil~ Akzo Nobel RP-18 (4.6 mm ID ~ 250 mm, 5 ~tm) column at an ambient temperature. Photo diode array detection was performed in program mode at 234 rim. The analyte and diazepam as internal standard (IS) were extracted from plasma using 10% trichloroacetic acid. The assay was linear over the therapeutic concentration range of 20-2,500 ng/mL for metformin HCI with correlation coefficient of r = 0.9999. Limit of quantitation was 20 ng/mL. The results obtained for intraJinter day accuracy and precision complied very well with the generally accepted criteria for bio-analytical assay. The method was applied to bioequivalence (BE) study of metformin HCI in healthy Indonesian volunteers after treatment with 750 mg XR metformin HCI. This BE study shows that the two formulations are equivalent so that they were therapeutically interchangeable for each other.展开更多
A reverse-phase HPLC-DAD method was developed for simultaneous quantification of ten phenolic acids (caffeic acid, chlorogenic acid, neochlorogenic acid, 4-O-caffeoylquinic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-di...A reverse-phase HPLC-DAD method was developed for simultaneous quantification of ten phenolic acids (caffeic acid, chlorogenic acid, neochlorogenic acid, 4-O-caffeoylquinic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid methyl ester, 3,4-O-dicaffeoylquinic acid methyl ester, and 4,5-0- dicaffeoylquinic acid methyl ester) in the dried flower buds of Lonicera japonica Thunb. (Lonicerae Japonicae Flos; LJF). An optimal sample preparation method was established as 30-min ultrasonication with 100 times 50% (v/w) ethanol aqueous solution based on the orthogonal test results. The chromatographic separation of the ten phenolic acids was achieved with an AQ-C18 column (4.6 mm x 250 mm, 5 p.m) and a gradient elution of acetonitrile, methanol and 0.1% formic acid aqueous solution within 55 rain. All calibration curves showed good linearity (r2〉0.999) within test ranges. The average recoveries were in the range of 98.57%-103.22% with RSD less than 3%. The method developed was accurate, sensitive and reproducible for determination of ten phenolic acids in LJF.展开更多
基金Project(20235020) supported by the National Natural Science Foundation of China
文摘The chemical components of the essential oils in the barks and leaves of Eucommia ulmoides Oliver were analyzed and compared by chromatograms and mass spectra technique, heuristic evolving latent projections (HELP), alternative moving window factor analysis (AMWFA) algorithms and normalization method based on the peak areas; the flavones in the barks and leaves of Eucommia ulmoides Oliver were separated on an ODS column by gradient elution carried out with the flow phase consisting of water, methanol and phosphoric acid (0.1%), and their contents were quantitatively determined by standard curve method and diode array detection (DAD) at 362 nm. The results show that 68 and 73 compounds respectively from essential oils of the barks and leaves of Eucommia ulmoides Oliver are identified, and there are 33 mutual compounds among 108 compounds determined. The total contents of these volatile components of the two samples possess 92.9% and 97.75% of the gross of the relevant essential oils, respectively; the contents of the rutin, quercetin and kaempferol in the barks and leaves of Eucommia ulmoides Oliver are 0.016 9, 0.003 6, 0.002 1 and 0.064 4, 0.030 2, 0.010 0 mg/g, respectively, and the determination recoveries are 95.2%-106.2%. The comparative analysis shows that for the barks and leaves of Eucommia ulmoides Oliver, there are significant differences in their components of the relevant essential oils and flavones.
基金Supported by Plan Issue of Shanghai Science &Technology Committee(No.13401901100)
文摘To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.
文摘This paper investigates the occurrence of sulphonamide and diaminopyrimidine antibiotics in wastewater and sludge from wastewater treatment plants. In our experiment, they were isolated from wastewater using the solid phase extraction method. In the case of sludge, pressurized solvent extraction techniques were used followed by solid phase extraction. The solid phase extraction method was used for purification and concentration. Sulphonamide and diaminopyrimidine antibiotics were determined using high performance liquid chromatography with diode-array detection. The selected antibiotics were determined in real sludge samples collected from the wastewater treatment plant in Brno-Mod^ice and in real wastewater samples collected from the wastewater treatment plant located on the grounds of the University of Veterinary and Pharmaceutical Sciences in Brno, using the developed and optimized method. Analyses showed that real samples of wastewater contained sulphathiazole 11.82μg/L at the inflow (7.1 μg/L at the outflow), sulphapyridine 18.57 I.tg/L (12.2 μg/L), sulphamethazine 13.52 μg/L (8.44 μg/L), sulphamethoxazole 14.06 lag/L (9.34 Ixg/L) and trimethoprim 521.4 lag/L (422.29 μg/L). Here it is demonstrated that drugs are removed through the wastewater treatment procedure only partially.
文摘Beer can be a rich source of phenolic acids in the diet. The present review summarizes the current state of work on phenolic acids in beer presented in the cited papers. In an overview, 10 hydroxybenzoic acids, three related aldehydes, two phenylacetic acids and eight hydroxycinnamic acids in beer are being reported. This review compares the phenolic acids content in alcoholic and non-alcoholic beers from Czech Republic, Germany, Italy, Austria and Poland, which had been examined by several authors. The quantification was achieved by HPLC with ultraviolet, diode array, coulometric array or fluorimetric detection. Ferulic acid is the main phenolic acid in all beers that had been studied, followed by p-coumaric, vanillic, caffeic, p-OH-benzoic and sinapic acids. Most of the phenolic acids in beer are present as bound forms and only a small portion can be detected as free compounds. The content of the phenolic acids in the non-alcoholic beers is lower than in the alcoholic beers mainly due to differences in the production process, yeast strains used, dealcoholization of beer etc..
文摘The crosstalk caused by oblique incident ray on a PIN detector array is analyzed. An integral expression of crosstalk factor in relation to incident angle and structure parameters is deduced and the correctness of the deduction is tested and verified.
文摘SEM-EDS (scanning electron microscopy-energy dispersive spectrometry) and HPLC (high performance liquid chromatography) with DAD (diode array detection) were used to examine metal-wrapped coloured textiles. The sample was provided from Azerbaijan History Museum. Material included silk and thin wire. SEM micrographs showed that the metal strip had 250μm width and 6 9m thickness. SEM-EDS results indicated elemental composition of the wrapping: the presence of gold, silver as the components of the gilt metals. Furthermore, sulphur and chlorine were determined as contaminants. EDS analysis also revealed that both sides were gildered. Colouring compounds in the same sample were identified by HPLC-DAD. The major colouring compound found in the red fibre sample in large quantity was carminic acid and fuchsin components. The presence of fuchsin, which is a synthetic dye, dates the sample between the end of 19th and beginning of 20th century. Fisetin, which is a natural dye, was detected in the yellow fibre.
文摘Petrovska klobasa is a traditional dry fermented sausage produced in the Autonomous Province of Vojvodina. Formation of nine hiogenic amines was determined in three sausage groups produced from hot deboned (A1) and cold meat (B1, B3) during drying and ripening in traditional room (A1, B1) and in industrial ripening chamber (B3). Dansyl chloride derived amines were analysed by high-performance liquid chromatography with diode-array detector (HPLC-DAD) on Eclipse XDB-C18 column. Histamine, the most important amine from food safety point of view, was not found in any of the analyzed samples. Serotonin and spermidine were also not detected in any samples, while spermin was determined in all analyzed samples. At the end of drying, phenylethylamine was the predominant amine in A1 sausage group (51.6 mg/kg), and tryptamine in B1 (38.1 mg/kg) and B3 (28.7 mg/kg) sausage groups. At the end of ripening, tryptamine was the predominant biogenic amine in all sausage groups (133, 121 and 39.8 mg/kg in A1, B1 and B3 groups, respectively). Total level of biogenic amines in all investigated sausages did not exceed 174 mg/kg at the end of drying and 238 mg/kg at the end of ripening period. Tryptamine and cadaverine may be used as indicators of total biogenic amines for sausages produced in traditional and indusrial conditions from hot deboned and cold meat.
文摘Zea mays L. is one of the biggest cropping systems among the sustainable development agronomy. Pollen from this crop source is unexplored and apiculture can be a good partner adding value to the product and creating new jobs helping to solve some social issues as unemployment. However, food safety is crucial, thus the aim of this study was to explore the flavonoid/phenolic profiles from Z. mays L. pollen as a fingerprint for this plant identification and also to demonstrate how the method of bee pollen samples (honeybee collected pollen) is applied. For this purpose, several sources ofZ. mays L. pollen were analyzed, including corn hybrids and genetic modified samples collected at the breeding fields. For this work, samples were taken at several years from 2000 to 2012 and collected from different countries and locations, such as Portugal, Mexico and Brazil. Results showed, for the first time, that the fingerprint (flavonoid/phenolic profile) for Z. mays L. pollen does not change over the time of sampling neither with the region of harvesting. The high performance liquid chromatography-diode array detector (HPLC/DAD) fingerprints of phenolic/flavonoid extract from Z. mays remain unchanged for all samples analyzed from different countries, hybrids and/or genetic modified plants. This is also the first study reporting these phenolic compounds not only in pollen collected directly from hybrid plants, but also in Z. mays bee pollen. The described fingerprinting method is easy, fast and accurate for the characterization of Z. mays L. pollen samples and complete microscopic analysis because it is species-specific.
文摘A sensitive and specific high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of metformin hydrochloride (HCI) in human plasma. The HPLC method consists of isocratic eluation with a mixture of 60% buffer (10 mM sodium dihyrogenphosphate-10 mM sodium dodecyl sulphate) and 40% acetonitrile with final pH 7.0 with flow rate of 1.0 mL/min on a Kromasil~ Akzo Nobel RP-18 (4.6 mm ID ~ 250 mm, 5 ~tm) column at an ambient temperature. Photo diode array detection was performed in program mode at 234 rim. The analyte and diazepam as internal standard (IS) were extracted from plasma using 10% trichloroacetic acid. The assay was linear over the therapeutic concentration range of 20-2,500 ng/mL for metformin HCI with correlation coefficient of r = 0.9999. Limit of quantitation was 20 ng/mL. The results obtained for intraJinter day accuracy and precision complied very well with the generally accepted criteria for bio-analytical assay. The method was applied to bioequivalence (BE) study of metformin HCI in healthy Indonesian volunteers after treatment with 750 mg XR metformin HCI. This BE study shows that the two formulations are equivalent so that they were therapeutically interchangeable for each other.
基金The National Key Technology R&D Program of China(Grant No.2011BAI07B082011BAI06B01)
文摘A reverse-phase HPLC-DAD method was developed for simultaneous quantification of ten phenolic acids (caffeic acid, chlorogenic acid, neochlorogenic acid, 4-O-caffeoylquinic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid methyl ester, 3,4-O-dicaffeoylquinic acid methyl ester, and 4,5-0- dicaffeoylquinic acid methyl ester) in the dried flower buds of Lonicera japonica Thunb. (Lonicerae Japonicae Flos; LJF). An optimal sample preparation method was established as 30-min ultrasonication with 100 times 50% (v/w) ethanol aqueous solution based on the orthogonal test results. The chromatographic separation of the ten phenolic acids was achieved with an AQ-C18 column (4.6 mm x 250 mm, 5 p.m) and a gradient elution of acetonitrile, methanol and 0.1% formic acid aqueous solution within 55 rain. All calibration curves showed good linearity (r2〉0.999) within test ranges. The average recoveries were in the range of 98.57%-103.22% with RSD less than 3%. The method developed was accurate, sensitive and reproducible for determination of ten phenolic acids in LJF.