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
Finely divided silver nanoparticles were synthesized via the hydrothermal method. Arabic gum （AG） was used as both the reductant and steric stabilizer without any other surfactant. By adjusting the reaction temperat...Finely divided silver nanoparticles were synthesized via the hydrothermal method. Arabic gum （AG） was used as both the reductant and steric stabilizer without any other surfactant. By adjusting the reaction temperature, mass ratio of AG to AgNO3, and reaction time, silver nanoparticles with different morphological characteristics could be obtained. The products were characterized by UV-Vis, FTIR, TEM, SEM, and XRD measurements. It was found that temperature and AG played an important role in the synthesis of mono-disperse silver nanoparticles. Well dispersed and quasispherical silver nanoparticles were obtained under the optimal synthesis conditions of 10 mmol/L AgNO3, m（AG）/m（AgN03）= l：1, 160 ℃ and 3 h.展开更多
Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extract...Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extracted from the dog serum using dichlromethane followed by derivatization with DNBF for 20 min at 100℃. The solvent was then evaporated at 60℃ under nitrogen, and the residue was taken up in 100 μL of mobile phase consisting of acetonitrile water (75∶30, v/v). The separation was performed on a Hypersil BDS C18 column with a flow rate of 0 8 mL·min -1 , and the ultraviolet detector wavelength was set at 350 nm. Results Extraction recovery ranged from 75.9% to 83.2%, and methodological recovery was between 96.5% and 109.3%. Within day RSD ranged from 1.5% to 6.3%, and inter day RSD was between 2 9% and 14.8%. The method showed good linearity (R=0.9998). Conclusion The method was simple, convenient and sensitive. The reaction of derivatization was reproducible.展开更多
Aim To investigate the active constituents responsible for thepharmacological activities of Angelica sinensis (Oliv) Diels. Methods Chromatography was used toisolate chemical components, and spectroscopy was used to i...Aim To investigate the active constituents responsible for thepharmacological activities of Angelica sinensis (Oliv) Diels. Methods Chromatography was used toisolate chemical components, and spectroscopy was used to identify their structures. Results Sevencompounds were isolated and their structures were identified as ferulic acid (1), conife-rylferukte(2) , bis (2-ethylhexyl) phthalate (3), dibutyl phthalate (4), lignoceric acid (5), palmitic acid(6), and Z-6, 7-cis-dihydroxyligustilide (7) Conclusion Bis (2-ethylhexyl) phthalate and dibutylphthalate were obtained from Angelica sinensis for the first time.展开更多
A pre-column derivatization HPLC method for the determination of peimine(P)and peiminine(PE)in Bulbus Fritillariae has been developed. Under the derivatization conditions optimized,the calibration curve is Y1=-3.83...A pre-column derivatization HPLC method for the determination of peimine(P)and peiminine(PE)in Bulbus Fritillariae has been developed. Under the derivatization conditions optimized,the calibration curve is Y1=-3.83×103+1.33 ×105X1,r=0.998 for P and Y2=-7.86 × 102+6.33 × 104X2,r=0995 for PE,where Y is the peak area and X is the weight of the alkaloid; the average recovery is 98.0%(n=5, RSD=2.1%) for P and 101.0%(n=5,RSD=4.1%)for PE,the linear range is from 0.504 μg to 3.126μg for P and from 0.520μgto 3.328μgfor PE,respectively. Results of the determination of the two alkaloids in several samples of different Fritillaria species from various parts ofthe country are presented.The results suggest that P and PE are two major chemical constituents in bulbs of different Fritillaria species,and that the method developed is generally appli-cable to the determination of the hydroxy group on aliphatic fused ring systems without steric hin-drance.展开更多
The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture...The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture of chloroform-n-heptane.2-(4-Hydrazinocarbonyl- phenyl)-4,5-diphenylimidazole (HCPI) was used as a fluorescent labelling reagent of the fatty acids. The labelling reaction was carried out at 30℃ for 1 h at pH 6.5 and the resulting reaction mixture was sudjected to HPLC. The labelled fatty acid C_(17)(P-C_(17))was used as the internal standard. The la- belled fatty acids C_(16) and C_(18) were separated within 18 min on an ODS-8OTM column (150 mm× 6 mm ID,5μm,Tosoh Japan).The calibrlation curves of fatty acids from the spiked control serum were Y_1=-0.003 7 + 0.0028X_1,r=0.994 for FA C_( 16) and Y_2=0.00 1 2 + 0.00098X_2,r=0.999 for FA C_( 18),respectively.The average recoveries of facids from the spiked contrl serum were 107.2%(n=8,RSD=4.3%)for FA C_(16) and 97.35%(n=8, RSD=4.0%)for FA C_(18),respectively.The lower detection limits of fatty acids after reaction were 12μmol per 20μl injection for FA C_(16) and 18 μmol per 20μl injection for FA C_(18),respectively(signal to noise ratio, S/N=2).The HPLC/CL method was applied to the determination of FA C_(16) and FA C_(18) in normal human serum and the results showed that the concentrations of fatty acids in normal human serum were 0.134 ± 0.009 μ mol/ml serum(n=5) for FA C_(16) and 0.052±0.028 μmol/ml serum(n=5)for FA C_(18),respectively.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
A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four...A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four clear group fractions and a nonpolar fraction. All the fractions were analyzed by GC/MS. A total of 204 compounds were detected from the original CDSSF and its further separated fractions, with 173 compounds more than those detected by studying the original CDSSF directly. The results demonstrate a clear group separation by column chromatography in coal organic components and a more accessibility to coal components compared with the solvent extraction only.展开更多
Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oil...Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.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Finely divided silver nanoparticles were synthesized via the hydrothermal method. Arabic gum （AG） was used as both the reductant and steric stabilizer without any other surfactant. By adjusting the reaction temperature, mass ratio of AG to AgNO3, and reaction time, silver nanoparticles with different morphological characteristics could be obtained. The products were characterized by UV-Vis, FTIR, TEM, SEM, and XRD measurements. It was found that temperature and AG played an important role in the synthesis of mono-disperse silver nanoparticles. Well dispersed and quasispherical silver nanoparticles were obtained under the optimal synthesis conditions of 10 mmol/L AgNO3, m（AG）/m（AgN03）= l：1, 160 ℃ and 3 h.
文摘Aim A simple, sensitive and rapid RP HPLC method with pre column derivatization has been developed for the determination of sulphonylurea glimepiride in dog serum. Methods The sulphonylurea glimepiride was extracted from the dog serum using dichlromethane followed by derivatization with DNBF for 20 min at 100℃. The solvent was then evaporated at 60℃ under nitrogen, and the residue was taken up in 100 μL of mobile phase consisting of acetonitrile water (75∶30, v/v). The separation was performed on a Hypersil BDS C18 column with a flow rate of 0 8 mL·min -1 , and the ultraviolet detector wavelength was set at 350 nm. Results Extraction recovery ranged from 75.9% to 83.2%, and methodological recovery was between 96.5% and 109.3%. Within day RSD ranged from 1.5% to 6.3%, and inter day RSD was between 2 9% and 14.8%. The method showed good linearity (R=0.9998). Conclusion The method was simple, convenient and sensitive. The reaction of derivatization was reproducible.
文摘Aim To investigate the active constituents responsible for thepharmacological activities of Angelica sinensis (Oliv) Diels. Methods Chromatography was used toisolate chemical components, and spectroscopy was used to identify their structures. Results Sevencompounds were isolated and their structures were identified as ferulic acid (1), conife-rylferukte(2) , bis (2-ethylhexyl) phthalate (3), dibutyl phthalate (4), lignoceric acid (5), palmitic acid(6), and Z-6, 7-cis-dihydroxyligustilide (7) Conclusion Bis (2-ethylhexyl) phthalate and dibutylphthalate were obtained from Angelica sinensis for the first time.
文摘A pre-column derivatization HPLC method for the determination of peimine(P)and peiminine(PE)in Bulbus Fritillariae has been developed. Under the derivatization conditions optimized,the calibration curve is Y1=-3.83×103+1.33 ×105X1,r=0.998 for P and Y2=-7.86 × 102+6.33 × 104X2,r=0995 for PE,where Y is the peak area and X is the weight of the alkaloid; the average recovery is 98.0%(n=5, RSD=2.1%) for P and 101.0%(n=5,RSD=4.1%)for PE,the linear range is from 0.504 μg to 3.126μg for P and from 0.520μgto 3.328μgfor PE,respectively. Results of the determination of the two alkaloids in several samples of different Fritillaria species from various parts ofthe country are presented.The results suggest that P and PE are two major chemical constituents in bulbs of different Fritillaria species,and that the method developed is generally appli-cable to the determination of the hydroxy group on aliphatic fused ring systems without steric hin-drance.
文摘The peroxyoxalate chemiluminescence(CL)detection of fatty acids in human se- rum combined with high-performance liquid chromatography (HPLC)is described.Some fatty acids in serum were extracted with a 1 :1(v/v)mixture of chloroform-n-heptane.2-(4-Hydrazinocarbonyl- phenyl)-4,5-diphenylimidazole (HCPI) was used as a fluorescent labelling reagent of the fatty acids. The labelling reaction was carried out at 30℃ for 1 h at pH 6.5 and the resulting reaction mixture was sudjected to HPLC. The labelled fatty acid C_(17)(P-C_(17))was used as the internal standard. The la- belled fatty acids C_(16) and C_(18) were separated within 18 min on an ODS-8OTM column (150 mm× 6 mm ID,5μm,Tosoh Japan).The calibrlation curves of fatty acids from the spiked control serum were Y_1=-0.003 7 + 0.0028X_1,r=0.994 for FA C_( 16) and Y_2=0.00 1 2 + 0.00098X_2,r=0.999 for FA C_( 18),respectively.The average recoveries of facids from the spiked contrl serum were 107.2%(n=8,RSD=4.3%)for FA C_(16) and 97.35%(n=8, RSD=4.0%)for FA C_(18),respectively.The lower detection limits of fatty acids after reaction were 12μmol per 20μl injection for FA C_(16) and 18 μmol per 20μl injection for FA C_(18),respectively(signal to noise ratio, S/N=2).The HPLC/CL method was applied to the determination of FA C_(16) and FA C_(18) in normal human serum and the results showed that the concentrations of fatty acids in normal human serum were 0.134 ± 0.009 μ mol/ml serum(n=5) for FA C_(16) and 0.052±0.028 μmol/ml serum(n=5)for FA C_(18),respectively.
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Projects 90410018 and 20676142 supported by the National Natural Science Foundation of China2004CB[26]7601 by the Special Fund for Major State Basic ResearchJHB05-33 by the Program of the Universities in Jiangsu Province for the Development of High-Tech Industries
文摘A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four clear group fractions and a nonpolar fraction. All the fractions were analyzed by GC/MS. A total of 204 compounds were detected from the original CDSSF and its further separated fractions, with 173 compounds more than those detected by studying the original CDSSF directly. The results demonstrate a clear group separation by column chromatography in coal organic components and a more accessibility to coal components compared with the solvent extraction only.
文摘Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.
