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.
The leaf structure, content and the storage location of aloin in the leaves of six species of Aloe L. were studied by means of semi-thin section, high performance liquid chromatography (HPLC) and fluorescent microscop...The leaf structure, content and the storage location of aloin in the leaves of six species of Aloe L. were studied by means of semi-thin section, high performance liquid chromatography (HPLC) and fluorescent microscope. Results showed that all leaves consisted of epidermis, chlorenchyma, aquiferous tissue and vascular bundles. The leaves had the xeromorphic characteristics, including thickened epidermal cell wall, thickened cuticle, sunken stomata and well-developed aquiferous tissue. With the exception of thus, there were remarkable differences in leaf structure among the six species. The chlorenchyma cells were similar to palisade tissues in Aloe arborescens Mill. and A. mutabilis Pillans, but isodiametric in A. vera L., A. vera L. var. chinensis Berg., A. saponaria Hawer and A. greenii Bali. A. arborescens, A. mutabilis, A. very and A. vera var. chinensis included large parenchymatous cells at the vascular bundles, whereas no such cells were observed at the vascular bundles of A. saponaria and A. greenii. In A. arborescens, A. mutabilis and A. vera, the aquiferous tissue sheaths were present and composed of a layer of small parenchymatous cells without chloroplasts around the aquiferous tissue. While there were no aquiferous tissue sheaths in A. vera var. chinensis, A. saponaria and A. greenii. The HPLC revealed that the content of aloin was high in A. arborescens, low in A. vera, and very low in A. saponaria among the six species. The fluorescent microscopy showed that the yellow-green globule only appeared in the large parenchymatous cells of vascular bundles, vascular bundle sheath and aquiferous tissue sheath, but not in the chlorenchyma and aquiferous tissue. Consequently, the large parenchymatous cells of vascular bundles, vascular bundle sheath and aquiferous tissue sheath were the storage location of aloin. They were positively correlated with the content of aloin.展开更多
Ahn To establish an RP-HPLC method for determination of content of 1-phenylpropanol in its raw material and preparations. Methods Chromatography was carried out on a Dikma DiamonsilTM ODS column, using a mobile phase ...Ahn To establish an RP-HPLC method for determination of content of 1-phenylpropanol in its raw material and preparations. Methods Chromatography was carried out on a Dikma DiamonsilTM ODS column, using a mobile phase of methanol-water (55:45) with a flow rate at 1.0 mL·min^-1. The detection wavelength was 258 nm. Results Under the chromatographic condition, the peaks of 1-phenylpropanol and its related impurities separated completely; noninterference between the principal agent and adjuvants in preparations was performed. The calibration curve was linear over the range of 250 - 750μg·mL^-1 with the correlation coefficient of 0. 999 9. The average recovery was 100.2% ( RSD = 1.35% ). Conclusion This method is simple, rapid, accurate, specific, and can be used to detect the content and related compounds of phenylpropanol in its raw material and preparations.展开更多
[Objective] This study aimed to extract magnolol from wild Magnolia offici- nalia leaves by ultrasonic-assisted extraction. [Method] Magnolol was qualitatively id- entified by coloration method and thin layer chromato...[Objective] This study aimed to extract magnolol from wild Magnolia offici- nalia leaves by ultrasonic-assisted extraction. [Method] Magnolol was qualitatively id- entified by coloration method and thin layer chromatography, and magnolol content in Magnolia officinalia leaves was measured by high performance liquid chromatog- raphy (HPLC). The HPLC was conducted with C18 as the stationary phase while different mobile phases were selected. The measurement wavelength, flow velocity and sample size adopted in the HPLC were 294 nm, 1 ml/min and 20 μl, respec- tively. [Result] Magnolol content in Magnolia officinalia leaves was 0.75%. When methyl alcohol and water with a volume ratio of 78:22 was used as the mobile phase, the retention time of magnolol was 4.528 min and the separation effect was good. In addition, it was easy to operate with good reproducibility and sensitivity. [Conclusion] This method is suitable for the measurement of magnolol content in Maonolia officinalia leaves.展开更多
Aim To establish a reversed phase liquid chromatographic method forsimultaneous determination of three main medicinal constituents, baicalin, berberine and rhein, inSanhuang tablets. Methods The separation was perform...Aim To establish a reversed phase liquid chromatographic method forsimultaneous determination of three main medicinal constituents, baicalin, berberine and rhein, inSanhuang tablets. Methods The separation was performed on a Kromasil C_(18) column with TEA-adjusted0.02 mol·L^(-1) H_3PO_4 (pH 6.78)-acetonitrile-methanol (40 : 9 : 7) as mobile phase at aflow-rate of 1.0 mL·min^(-1), with detection at 254 ran. Considering interaction between acidic andalkaline compounds, three standard markers were added respectively and the volume of samplesolution was doubled in recovery experiments. Results Three regression equations revealed excellentlinear relationship between the peak areas and concentrations and the correlation coefficients allsurpassed 0.999 8. The average recovery was 96.1% (RSD = 2.1%) baicalin, 98.5% (RSD = 2.4%) forberberine, and 101.5% (RSD =1.3%) for rhein. Conclusion The method developed can be used to controlthe quality of Sanhuang tablets comprehensively.展开更多
[Objective] This study aimed to analyze the interaction between genotype of flavonoids of barley grain and environment, to increase the flavonoid content of barley grain in cultivation and breeding. [Method] In this s...[Objective] This study aimed to analyze the interaction between genotype of flavonoids of barley grain and environment, to increase the flavonoid content of barley grain in cultivation and breeding. [Method] In this study, the content of cate- chin, myricetin, quercetin and kaempferol of barley grain planted in Kunming, Qujing and Baoshan were determined by HPLC, and the genotype, environment, genotype- environment interaction of the flavonoid content of barley grain were analyzed. [Result] According to the experimental results, the genotype variance, environmental variance and G x E interaction variance of catechin and kaempferol contents show the same trend: genotype variation 〉 environmental variation 〉 G × E interaction variation, which all reach a extremely significant level; the genotype variance, envi- ronmental variance and G × E interaction variance of quercetin and total flavonoid contents show the same trend: genetype variation 〉 G × E interaction variation 〉 environmental variation, which all reach a extremely significant level; the genotype variance and environmental variance of myricetin content both reach a extremely sig- nificant level, while the G × E interaction variance reaches a significant level, showing an order of genotype variation 〉 environmental variation 〉 G × E interaction variation; the genotype variance, environmental variance and G x E interaction vari- ance of total flavonoid content show an order of genotype variation 〉 environmental variation 〉 G × E interaction variation. Among different barley varieties, Ziguang- mangluoerling and Kuanyingdamai in Qujing, Kunming and Baoshan have relatively high content of quercetin, while other barley varieties barely contain any quercetin. The grains of Ziguangmangluoerling and Kuanyingdamai are purple, while the grains of other barley varieties are yellow. [Conclusion] Four main flavonoids and the total flavonoids of barley grain are mainly under genetic control and affected by genetic- environment interactions; the purple barley grains contain high content of quercetin.展开更多
[Objective] The aim was to establish an HPLC method for determination of phytoene content in tomato ketchup. [Method] The chromatographic conditions were as follows: column, Agilent AT C18 (250 mm×4.6 mm, 5 μm...[Objective] The aim was to establish an HPLC method for determination of phytoene content in tomato ketchup. [Method] The chromatographic conditions were as follows: column, Agilent AT C18 (250 mm×4.6 mm, 5 μm); mobile phase, methanol-THF (75:25); detection wavelength, 287 nm; flow rate, 1.0 ml/min; column temperature, 30 ℃; sample size, 50 μl. [Result] There was a good linear relation- ship in the phytoene content range of 0.186-1.116μg. The average recovery rate was 103.8% with RSD of 1.47%. The phytoene content in the tomato ketchup sample was determined as 10.7 rag/100 g simple, accurate, rapid and reliable, and phytoene content in tomato ketchup. [Conclusion] The established method is it can be used for the determination of展开更多
Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS col...Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.展开更多
A reserved-phase HPLC method was developed for the determination of barbaloin in Aloe vera L. var. chinensis (Haw.) Berger and Aloe barbadensis Miller, and whether there was a close relationship between the contents o...A reserved-phase HPLC method was developed for the determination of barbaloin in Aloe vera L. var. chinensis (Haw.) Berger and Aloe barbadensis Miller, and whether there was a close relationship between the contents of barbaloin and their environments in which they were growing was decided. A Hypersil ODS column (4.6 mm×200 mm, 5 μm)was used with a mobile phase of methanol-water (40:60, containing 0.1% acetic acid), the flow rate being 1.0 mL·min -1, detection wavelength at 359 nm, and the column temperature being 30℃. The linear range of barbaloin was between 0.0726 and 0.726 μg with a correlation coefficient of 0.9998 and the regression equation being Y=1.9202×10 6X-1801.9. Barbaloin was stable in methanol in 48 h and the instrument precision was 1.2% while the method precision was 4.9%. The contents of barbaloin of 12 samples ranged from 6.160 to 319.1 μg·g -1. The method developed was fast and simple with good reproducibility. There was high correlation between the contents of barbaloin and their growing environments.展开更多
A gradient HPLC method was established for the determination of harpagoside and cinnamic acid in Radix Scrophulariae (Xuanshen) and a proposition was put forward for the lowest content of the characteristic and active...A gradient HPLC method was established for the determination of harpagoside and cinnamic acid in Radix Scrophulariae (Xuanshen) and a proposition was put forward for the lowest content of the characteristic and active constituent (harpagoside) for qualified Radix Scrophulariae. The experimental conditions were as follows: Ultrasphere ODS column (250 mm 4.6 mm, 5 mm), mobile phase: acetonitrile-water (containing 1.0% acetic acid) (20:8050:50) (20 min), flow-rate 1 mLmin-1, room temperature, detection wavelength 278 nm. Twenty-eight samples of Xuan-shen (Radix Scrophulariae) from different districts of China were analyzed and the contents of harpagoside and cinnamic acid in Xuan-shen were 0.041~0.244% and 0.012~0.068% respectively. The recoveries (RSD)% were 97.13(0.80)% for harpagoside and 99.38(0.51)% for cinnamic acid. The method is simple and accurate. It can be used for the quality control of Radix Scrophulariae. We propose that the content of harpagoside in qualified Radix Scrophularia should be no less than 0.05%.展开更多
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
The property of the contact surface between geosynthetics and soil directly affects the whole structure's stability. The interface property is one of the most important indices for the reinforced structure. Systemati...The property of the contact surface between geosynthetics and soil directly affects the whole structure's stability. The interface property is one of the most important indices for the reinforced structure. Systematic direct-shear tests with large direct-shear apparatus are carded out for geobelt reinforced clay under different normal stresses and water content. A reinforcement-sand-clay layer system improving the interface behavior greatly is designed. The stress-strain relationship is investigated on the basis of the experimental results. The results show that with the increase of the normal stress, the shear strength between the clay and the reinforcement increases nonlinearly, and with the increase of the water content, the friction coefficient between the clay and the reinforcement decreases dramatically and the cohesion between the clay and the polypropylene geobelt increases initially, then decreases. There is an optimal value for the water content between the clay and the polypropylene geobelt, which is 2% lower than the optimal water content of clay compaction. This reinforcement-sand-clay layer system improves the shear strength of the interface remarkably. Therefore, the clay-sand-reinforcement layer system is a rather good design for practical use in reinforcement engineering.展开更多
A silicone oil emulsion with 60% of solid content was prepared with methyl silicone oil used as the main material by means of the emulsifier-in-oil method.The influence of emulsification conditions on the droplet diam...A silicone oil emulsion with 60% of solid content was prepared with methyl silicone oil used as the main material by means of the emulsifier-in-oil method.The influence of emulsification conditions on the droplet diameter of silicone oil emulsion was discussed.The experimental results showed that the emulsification method,including the quantity of the emulsifier,the time and temperature of emulsification,the emulsifying water dosage,and the stirring speed,had significant impact on the droplet size.The optimal conditions were identified to achieve a smallest droplet diameter of the emulsion at an emulsifier dosage of 6%,an emulsification temperature of 70 ℃,an emulsification time of 30 min,and a stirring speed of 1100 r/min,with water added in two portions at a ratio of 1:1.The high-solid content silicone oil emulsion with a mean droplet diameter of 2.731 μm was prepared under these conditions that could ensure absence of stratification and floating oil under centrifuging at a speed of 3000 r/min for 30 min.展开更多
In order to study the hydrolytic characterization of an anti-inflammatory prodrug ( RI-1 ) in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolyti...In order to study the hydrolytic characterization of an anti-inflammatory prodrug ( RI-1 ) in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography (RP-HPLC). The chromatographic separation is performed on an ODS-2 C18 column (250 mm × 4. 6 mm, 5.0 μm particle size) with a simple elution program. The mobile phase is V( methanol) : V(0. 1% phosphoric acid solution) =90:10 (adjust pH to 2. 3). A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.展开更多
The non-random two liquids (NRTL) equation together with the Pitzer/Curl Virial equation of state are used to investigate the simultaneous representation of excess enthalpies (h^E) and vapour-liquid equilibria (...The non-random two liquids (NRTL) equation together with the Pitzer/Curl Virial equation of state are used to investigate the simultaneous representation of excess enthalpies (h^E) and vapour-liquid equilibria (VLE) and the VLE prediction from h^E data. The calculation strategy for properly determining NRTL parameters and the effect of their temperature dependence on the simultaneous correlation of h^E and VLE data and the VLE extrapolation are analysed in detail.展开更多
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The leaf structure, content and the storage location of aloin in the leaves of six species of Aloe L. were studied by means of semi-thin section, high performance liquid chromatography (HPLC) and fluorescent microscope. Results showed that all leaves consisted of epidermis, chlorenchyma, aquiferous tissue and vascular bundles. The leaves had the xeromorphic characteristics, including thickened epidermal cell wall, thickened cuticle, sunken stomata and well-developed aquiferous tissue. With the exception of thus, there were remarkable differences in leaf structure among the six species. The chlorenchyma cells were similar to palisade tissues in Aloe arborescens Mill. and A. mutabilis Pillans, but isodiametric in A. vera L., A. vera L. var. chinensis Berg., A. saponaria Hawer and A. greenii Bali. A. arborescens, A. mutabilis, A. very and A. vera var. chinensis included large parenchymatous cells at the vascular bundles, whereas no such cells were observed at the vascular bundles of A. saponaria and A. greenii. In A. arborescens, A. mutabilis and A. vera, the aquiferous tissue sheaths were present and composed of a layer of small parenchymatous cells without chloroplasts around the aquiferous tissue. While there were no aquiferous tissue sheaths in A. vera var. chinensis, A. saponaria and A. greenii. The HPLC revealed that the content of aloin was high in A. arborescens, low in A. vera, and very low in A. saponaria among the six species. The fluorescent microscopy showed that the yellow-green globule only appeared in the large parenchymatous cells of vascular bundles, vascular bundle sheath and aquiferous tissue sheath, but not in the chlorenchyma and aquiferous tissue. Consequently, the large parenchymatous cells of vascular bundles, vascular bundle sheath and aquiferous tissue sheath were the storage location of aloin. They were positively correlated with the content of aloin.
文摘Ahn To establish an RP-HPLC method for determination of content of 1-phenylpropanol in its raw material and preparations. Methods Chromatography was carried out on a Dikma DiamonsilTM ODS column, using a mobile phase of methanol-water (55:45) with a flow rate at 1.0 mL·min^-1. The detection wavelength was 258 nm. Results Under the chromatographic condition, the peaks of 1-phenylpropanol and its related impurities separated completely; noninterference between the principal agent and adjuvants in preparations was performed. The calibration curve was linear over the range of 250 - 750μg·mL^-1 with the correlation coefficient of 0. 999 9. The average recovery was 100.2% ( RSD = 1.35% ). Conclusion This method is simple, rapid, accurate, specific, and can be used to detect the content and related compounds of phenylpropanol in its raw material and preparations.
基金Industrialization Cultivation Project of Shaanxi Province Education Department(2012JC09)Scientific and Technological Project of Social Development of Shaanxi Science and Technology Agency(2015SF270)~~
文摘[Objective] This study aimed to extract magnolol from wild Magnolia offici- nalia leaves by ultrasonic-assisted extraction. [Method] Magnolol was qualitatively id- entified by coloration method and thin layer chromatography, and magnolol content in Magnolia officinalia leaves was measured by high performance liquid chromatog- raphy (HPLC). The HPLC was conducted with C18 as the stationary phase while different mobile phases were selected. The measurement wavelength, flow velocity and sample size adopted in the HPLC were 294 nm, 1 ml/min and 20 μl, respec- tively. [Result] Magnolol content in Magnolia officinalia leaves was 0.75%. When methyl alcohol and water with a volume ratio of 78:22 was used as the mobile phase, the retention time of magnolol was 4.528 min and the separation effect was good. In addition, it was easy to operate with good reproducibility and sensitivity. [Conclusion] This method is suitable for the measurement of magnolol content in Maonolia officinalia leaves.
基金Innovation Fund of Chinese Academy of Sciences(KGCX2 SW 213 05)
文摘Aim To establish a reversed phase liquid chromatographic method forsimultaneous determination of three main medicinal constituents, baicalin, berberine and rhein, inSanhuang tablets. Methods The separation was performed on a Kromasil C_(18) column with TEA-adjusted0.02 mol·L^(-1) H_3PO_4 (pH 6.78)-acetonitrile-methanol (40 : 9 : 7) as mobile phase at aflow-rate of 1.0 mL·min^(-1), with detection at 254 ran. Considering interaction between acidic andalkaline compounds, three standard markers were added respectively and the volume of samplesolution was doubled in recovery experiments. Results Three regression equations revealed excellentlinear relationship between the peak areas and concentrations and the correlation coefficients allsurpassed 0.999 8. The average recovery was 96.1% (RSD = 2.1%) baicalin, 98.5% (RSD = 2.4%) forberberine, and 101.5% (RSD =1.3%) for rhein. Conclusion The method developed can be used to controlthe quality of Sanhuang tablets comprehensively.
基金Supported by National Barley Industrial Technology System of China(CARS-05)National Natural Science Foundation of China(No.31260326)~~
文摘[Objective] This study aimed to analyze the interaction between genotype of flavonoids of barley grain and environment, to increase the flavonoid content of barley grain in cultivation and breeding. [Method] In this study, the content of cate- chin, myricetin, quercetin and kaempferol of barley grain planted in Kunming, Qujing and Baoshan were determined by HPLC, and the genotype, environment, genotype- environment interaction of the flavonoid content of barley grain were analyzed. [Result] According to the experimental results, the genotype variance, environmental variance and G x E interaction variance of catechin and kaempferol contents show the same trend: genotype variation 〉 environmental variation 〉 G × E interaction variation, which all reach a extremely significant level; the genotype variance, envi- ronmental variance and G × E interaction variance of quercetin and total flavonoid contents show the same trend: genetype variation 〉 G × E interaction variation 〉 environmental variation, which all reach a extremely significant level; the genotype variance and environmental variance of myricetin content both reach a extremely sig- nificant level, while the G × E interaction variance reaches a significant level, showing an order of genotype variation 〉 environmental variation 〉 G × E interaction variation; the genotype variance, environmental variance and G x E interaction vari- ance of total flavonoid content show an order of genotype variation 〉 environmental variation 〉 G × E interaction variation. Among different barley varieties, Ziguang- mangluoerling and Kuanyingdamai in Qujing, Kunming and Baoshan have relatively high content of quercetin, while other barley varieties barely contain any quercetin. The grains of Ziguangmangluoerling and Kuanyingdamai are purple, while the grains of other barley varieties are yellow. [Conclusion] Four main flavonoids and the total flavonoids of barley grain are mainly under genetic control and affected by genetic- environment interactions; the purple barley grains contain high content of quercetin.
基金Supported by Special Fund for Small and Medium Enterprises of Shihezi in the Eighth Division of Xinjiang Production and Construction Corps(2013QY16)~~
文摘[Objective] The aim was to establish an HPLC method for determination of phytoene content in tomato ketchup. [Method] The chromatographic conditions were as follows: column, Agilent AT C18 (250 mm×4.6 mm, 5 μm); mobile phase, methanol-THF (75:25); detection wavelength, 287 nm; flow rate, 1.0 ml/min; column temperature, 30 ℃; sample size, 50 μl. [Result] There was a good linear relation- ship in the phytoene content range of 0.186-1.116μg. The average recovery rate was 103.8% with RSD of 1.47%. The phytoene content in the tomato ketchup sample was determined as 10.7 rag/100 g simple, accurate, rapid and reliable, and phytoene content in tomato ketchup. [Conclusion] The established method is it can be used for the determination of
文摘Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.
文摘A reserved-phase HPLC method was developed for the determination of barbaloin in Aloe vera L. var. chinensis (Haw.) Berger and Aloe barbadensis Miller, and whether there was a close relationship between the contents of barbaloin and their environments in which they were growing was decided. A Hypersil ODS column (4.6 mm×200 mm, 5 μm)was used with a mobile phase of methanol-water (40:60, containing 0.1% acetic acid), the flow rate being 1.0 mL·min -1, detection wavelength at 359 nm, and the column temperature being 30℃. The linear range of barbaloin was between 0.0726 and 0.726 μg with a correlation coefficient of 0.9998 and the regression equation being Y=1.9202×10 6X-1801.9. Barbaloin was stable in methanol in 48 h and the instrument precision was 1.2% while the method precision was 4.9%. The contents of barbaloin of 12 samples ranged from 6.160 to 319.1 μg·g -1. The method developed was fast and simple with good reproducibility. There was high correlation between the contents of barbaloin and their growing environments.
文摘A gradient HPLC method was established for the determination of harpagoside and cinnamic acid in Radix Scrophulariae (Xuanshen) and a proposition was put forward for the lowest content of the characteristic and active constituent (harpagoside) for qualified Radix Scrophulariae. The experimental conditions were as follows: Ultrasphere ODS column (250 mm 4.6 mm, 5 mm), mobile phase: acetonitrile-water (containing 1.0% acetic acid) (20:8050:50) (20 min), flow-rate 1 mLmin-1, room temperature, detection wavelength 278 nm. Twenty-eight samples of Xuan-shen (Radix Scrophulariae) from different districts of China were analyzed and the contents of harpagoside and cinnamic acid in Xuan-shen were 0.041~0.244% and 0.012~0.068% respectively. The recoveries (RSD)% were 97.13(0.80)% for harpagoside and 99.38(0.51)% for cinnamic acid. The method is simple and accurate. It can be used for the quality control of Radix Scrophulariae. We propose that the content of harpagoside in qualified Radix Scrophularia should be no less than 0.05%.
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The property of the contact surface between geosynthetics and soil directly affects the whole structure's stability. The interface property is one of the most important indices for the reinforced structure. Systematic direct-shear tests with large direct-shear apparatus are carded out for geobelt reinforced clay under different normal stresses and water content. A reinforcement-sand-clay layer system improving the interface behavior greatly is designed. The stress-strain relationship is investigated on the basis of the experimental results. The results show that with the increase of the normal stress, the shear strength between the clay and the reinforcement increases nonlinearly, and with the increase of the water content, the friction coefficient between the clay and the reinforcement decreases dramatically and the cohesion between the clay and the polypropylene geobelt increases initially, then decreases. There is an optimal value for the water content between the clay and the polypropylene geobelt, which is 2% lower than the optimal water content of clay compaction. This reinforcement-sand-clay layer system improves the shear strength of the interface remarkably. Therefore, the clay-sand-reinforcement layer system is a rather good design for practical use in reinforcement engineering.
文摘A silicone oil emulsion with 60% of solid content was prepared with methyl silicone oil used as the main material by means of the emulsifier-in-oil method.The influence of emulsification conditions on the droplet diameter of silicone oil emulsion was discussed.The experimental results showed that the emulsification method,including the quantity of the emulsifier,the time and temperature of emulsification,the emulsifying water dosage,and the stirring speed,had significant impact on the droplet size.The optimal conditions were identified to achieve a smallest droplet diameter of the emulsion at an emulsifier dosage of 6%,an emulsification temperature of 70 ℃,an emulsification time of 30 min,and a stirring speed of 1100 r/min,with water added in two portions at a ratio of 1:1.The high-solid content silicone oil emulsion with a mean droplet diameter of 2.731 μm was prepared under these conditions that could ensure absence of stratification and floating oil under centrifuging at a speed of 3000 r/min for 30 min.
文摘In order to study the hydrolytic characterization of an anti-inflammatory prodrug ( RI-1 ) in vitro, an effective, accurate and reliable method for the simultaneous determination of the prodrug and its two hydrolytic active compounds is developed using reverse phase high-performance liquid chromatography (RP-HPLC). The chromatographic separation is performed on an ODS-2 C18 column (250 mm × 4. 6 mm, 5.0 μm particle size) with a simple elution program. The mobile phase is V( methanol) : V(0. 1% phosphoric acid solution) =90:10 (adjust pH to 2. 3). A wavelength of 225 nm and a mobile phase flow rate of 1.0 mL/min are utilized for the quantitative analysis. Excellent linear behaviors over the investigated concentration ranges are observed with values of R2 higher than 0. 999 for all the analytes. The validated method is successfully applied to the simultaneous determination of the prodrug and its active components can be used to detect hydrolytic characterization in vitro.
基金Supported by Deutsche Forschungsgemeinschaft(DFG) (LE 886/4-1)
文摘The non-random two liquids (NRTL) equation together with the Pitzer/Curl Virial equation of state are used to investigate the simultaneous representation of excess enthalpies (h^E) and vapour-liquid equilibria (VLE) and the VLE prediction from h^E data. The calculation strategy for properly determining NRTL parameters and the effect of their temperature dependence on the simultaneous correlation of h^E and VLE data and the VLE extrapolation are analysed in detail.