A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.Afte...A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.After shell is dried,organics from shrimp shell are extracted with anhydrous ethanol.The alcohol extrative of the shrimp shell is mixed with the ammonium sulfate to extract astaxanthin by aqueous two-phase extraction.The crude astaxanthin is collected,which is distributed in the middle layer of the aqueous two-phase layer.After distilled water is added to the crude astaxanthin,the aqueous solution is centrifuged,and the previous step is repeated for several times.The precipitation in centrifuge tube is collected and dried.The crude astaxanthin dried is dissolved with acetone,and the sample solution is separated by TLC.Every pigment on the TLC plate is collected and dissolved with acetone.The pigments are determined by high performance liquid chromatograph.The results show that aqueous two-phase system,3 mL alcohol extractive of astaxanthin and 4.5 mL 20%ammonium sulfate,can be used to acquire crude astaxanthin.The wavelength of the maximum peak of astaxanthin in ethanol solution is 472 nm.A variety of pigments can be separated from the crude astaxanthin by thin-layer chromatography,including free astaxanthin,astaxanthin monoester,astaxanthin diester,echinenone and other substances.It can be seen from high performance liquid chromatography that the appearance time of free astaxanthin is from 4 min to 5.5 min,and the appearance time of astaxanthin monoester is from 10.5 min to 27.8 min.The method is simple about the sample pretreatment and feasible about the determination of astaxanthin and astaxanthin esters in shrimp shell.展开更多
[Objective] The aim was to conduct HPLC analysis on Cordyceps Sinensis/Betaine compound feed nutriment. [Method] Cordyceps Sinensis/Betaine compound feed nutriment was under HPLC analysis to determine separation of Co...[Objective] The aim was to conduct HPLC analysis on Cordyceps Sinensis/Betaine compound feed nutriment. [Method] Cordyceps Sinensis/Betaine compound feed nutriment was under HPLC analysis to determine separation of Cordyceps Sinensis effluent and betaine. [Result] Different compositions in Cordyceps Sinensis/etaine compound feed nutriment would be well separated by the method. [Conclusion] The method provides a suitable platform of separation and analysis for Cordyceps Sinensis /Betaine compound feed nutriment.展开更多
A promising bacterial strain for the biodegradation of Microcystins(MCs)was isolated from Dianchi lake in China and identified as Sphingopyxis sp.USTB-05 by the analysis of 16s rDNA.Initial MC-RR of 42.3 mg·L -1 ...A promising bacterial strain for the biodegradation of Microcystins(MCs)was isolated from Dianchi lake in China and identified as Sphingopyxis sp.USTB-05 by the analysis of 16s rDNA.Initial MC-RR of 42.3 mg·L -1 was completely degraded by USTB-05 within 36 h,which was a relatively high biodegradation rate of MC-RR.With the cell-free extract(CE)of Sphingopyxis sp.USTB-05,MC-RR was biodegraded at a more rapid biodegradation rate compared with its strain,so that initial MC-RR of 42.3 mg·L -1 was completely biodegraded within 10 h.During the bio-reaction of MC-RR catalyzed by CE,two intermediate metabolites and a dead-end product of MC-RR were observed on HPLC profiles and all of them had similar scanning profiles in the wavelength from 200 to 300 nm,indicating that the group of Adda in all products of MC-RR remained intact.展开更多
Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for t...Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.展开更多
The phosphate solubilizing characteristics of a strain YC, which was isolated from phosphate mines (Hubei, China), were studied in National Botanical Research Institute’s phosphate (NBRIP) growth medium containing tr...The phosphate solubilizing characteristics of a strain YC, which was isolated from phosphate mines (Hubei, China), were studied in National Botanical Research Institute’s phosphate (NBRIP) growth medium containing tricalcium phosphate (TCP) as sole phosphorus (P) source. The strain YC is identified as Stenotrophomonas maltophilia (S. maltophilia) based upon the results of morphologic, physiological and biochemical characteristics and 16S rRNA sequences analysis. The results show that the strain S. maltophilia YC can solubilize TCP and release soluble P in NBRIP growth medium. A positive correlation between concentration of soluble P and population of the isolate and a negative correlation between concentration of soluble P and pH in the culture medium are observed from statistical analysis results. Moreover, gluconic acid is detected in the culture medium by HPLC analysis. It indicates that the isolate can release gluconic acid during the solubilizing experiment, which causes acidification of the culture medium and then TCP solubilization. S. maltophilia YC has a maximal TCP solubilizing capability when using maltose as carbon source and ammonium nitrate as nitrogen source, respectively, in NBRIP growth medium.展开更多
Ibuprofen is widely used as a non-steroidal anti-inflammatory drug and produced as racemic mixture. Its pharmacological activity resides only in S-(+)-enantiomer, and R-()-enantiomer is not only inactive but also has ...Ibuprofen is widely used as a non-steroidal anti-inflammatory drug and produced as racemic mixture. Its pharmacological activity resides only in S-(+)-enantiomer, and R-()-enantiomer is not only inactive but also has many side effects. Thus it is necessary to separate R-enantiomer from racemic ibuprofen. We studied optical separation of racemic Ibuprofen with chiral high performance liquid chromatography (HPLC). Out of three different chiral stationary phases, which were selected on the basis of structure and availability, two were found to be ef-fective. There was optimum eluent composition for each stationary phase for good resolution in optical separation. Resolution decreased with increase of eluent flow rate, but effect of injection volume on resolution was insignificant at high eluent flow rate.展开更多
Irbesartan is an antihypertensive drug whose concentration in blood is very small so it requires a sensitive method of analysis, selective and valid for analysis. In this study, it is carried out optimization of analy...Irbesartan is an antihypertensive drug whose concentration in blood is very small so it requires a sensitive method of analysis, selective and valid for analysis. In this study, it is carried out optimization of analytical conditions and validation for the analysis of irbesartan in plasma. Chromatography was performed on a C 18 column （250 × 4.6 mm, 5 μm） under isocratic elution with acetonitrile-0.1% formic acid （46：54 v/v）, pH 3.75. Detection was made at excitation 250 nm and emission 370 nm and analyses were run at a flow-rate of 1.0 mL/min at a temperature of 40 ℃. Losartan potassium was used as internal standard. Plasma extraction was done by deproteination with acetonitrile, mixed with vortex for 30 seconds, then centrifuged it at 10,000 rpm for 10 rain. In plasma validation, the recovery was 96.22%, and the lower limit of quantification （LLOQ） in plasma was 2 ng/mL. The method also fulfill the criteria for accuracy and precision intra and inter day by normal values （%Diff） not exceed ± 15%. On the stability study, irbesartan in plasma temperature -20 ℃has been stable for 28 days.展开更多
基金supported by Liao Ning Revitalization Talents Program No. XLYC1807161Dalian High-level Talents Innovation Support Plan No. 2017RQ063+4 种基金Dalian Ocean University Zhanlan scholar ProgramThe National Natural Science Foundation of China under contract Nos. 41206013, 41430963the Public Science and Technology Research Funds Projects of Ocean under contract No. 201205018the National Science and Technology Support Program under contract No. 2014BAB12B02Projects of Institute of Marine Industry Technology of Liaoning Universities
文摘A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.After shell is dried,organics from shrimp shell are extracted with anhydrous ethanol.The alcohol extrative of the shrimp shell is mixed with the ammonium sulfate to extract astaxanthin by aqueous two-phase extraction.The crude astaxanthin is collected,which is distributed in the middle layer of the aqueous two-phase layer.After distilled water is added to the crude astaxanthin,the aqueous solution is centrifuged,and the previous step is repeated for several times.The precipitation in centrifuge tube is collected and dried.The crude astaxanthin dried is dissolved with acetone,and the sample solution is separated by TLC.Every pigment on the TLC plate is collected and dissolved with acetone.The pigments are determined by high performance liquid chromatograph.The results show that aqueous two-phase system,3 mL alcohol extractive of astaxanthin and 4.5 mL 20%ammonium sulfate,can be used to acquire crude astaxanthin.The wavelength of the maximum peak of astaxanthin in ethanol solution is 472 nm.A variety of pigments can be separated from the crude astaxanthin by thin-layer chromatography,including free astaxanthin,astaxanthin monoester,astaxanthin diester,echinenone and other substances.It can be seen from high performance liquid chromatography that the appearance time of free astaxanthin is from 4 min to 5.5 min,and the appearance time of astaxanthin monoester is from 10.5 min to 27.8 min.The method is simple about the sample pretreatment and feasible about the determination of astaxanthin and astaxanthin esters in shrimp shell.
文摘[Objective] The aim was to conduct HPLC analysis on Cordyceps Sinensis/Betaine compound feed nutriment. [Method] Cordyceps Sinensis/Betaine compound feed nutriment was under HPLC analysis to determine separation of Cordyceps Sinensis effluent and betaine. [Result] Different compositions in Cordyceps Sinensis/etaine compound feed nutriment would be well separated by the method. [Conclusion] The method provides a suitable platform of separation and analysis for Cordyceps Sinensis /Betaine compound feed nutriment.
基金Supported by the State Key Development Program for Basic Research of China（2008CB418105） the National Natural Science Foundation of China（203777008 20621703）+1 种基金 the State Key Joint Laboratory of Environment Simulation and Pollution Control（09K08ESPCT） the Educational Committee of Beijing
文摘A promising bacterial strain for the biodegradation of Microcystins(MCs)was isolated from Dianchi lake in China and identified as Sphingopyxis sp.USTB-05 by the analysis of 16s rDNA.Initial MC-RR of 42.3 mg·L -1 was completely degraded by USTB-05 within 36 h,which was a relatively high biodegradation rate of MC-RR.With the cell-free extract(CE)of Sphingopyxis sp.USTB-05,MC-RR was biodegraded at a more rapid biodegradation rate compared with its strain,so that initial MC-RR of 42.3 mg·L -1 was completely biodegraded within 10 h.During the bio-reaction of MC-RR catalyzed by CE,two intermediate metabolites and a dead-end product of MC-RR were observed on HPLC profiles and all of them had similar scanning profiles in the wavelength from 200 to 300 nm,indicating that the group of Adda in all products of MC-RR remained intact.
基金Project(20235010) support by the NSFC-KOSEF Scientific Cooperation ProgramProject supported by the Program for New Century Talents of University in Henan ProvinceProgram for Backbone Teacher in Henan Province, China
文摘Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.
基金Project(2004CB619201) supported by the Major State Basic Research and Development Program of ChinaProject(Z200515002) supported by the Key Project Foundation of the Education Department of Hubei Province, China+1 种基金Project(GCP200801) supported by the Open Research Fund of Key Laboratory for Green Chemical Process of Ministry of Education, ChinaProject(Q200811) supported by the Youths Science Foundation of Wuhan Institute of Technology, China
文摘The phosphate solubilizing characteristics of a strain YC, which was isolated from phosphate mines (Hubei, China), were studied in National Botanical Research Institute’s phosphate (NBRIP) growth medium containing tricalcium phosphate (TCP) as sole phosphorus (P) source. The strain YC is identified as Stenotrophomonas maltophilia (S. maltophilia) based upon the results of morphologic, physiological and biochemical characteristics and 16S rRNA sequences analysis. The results show that the strain S. maltophilia YC can solubilize TCP and release soluble P in NBRIP growth medium. A positive correlation between concentration of soluble P and population of the isolate and a negative correlation between concentration of soluble P and pH in the culture medium are observed from statistical analysis results. Moreover, gluconic acid is detected in the culture medium by HPLC analysis. It indicates that the isolate can release gluconic acid during the solubilizing experiment, which causes acidification of the culture medium and then TCP solubilization. S. maltophilia YC has a maximal TCP solubilizing capability when using maltose as carbon source and ammonium nitrate as nitrogen source, respectively, in NBRIP growth medium.
文摘Ibuprofen is widely used as a non-steroidal anti-inflammatory drug and produced as racemic mixture. Its pharmacological activity resides only in S-(+)-enantiomer, and R-()-enantiomer is not only inactive but also has many side effects. Thus it is necessary to separate R-enantiomer from racemic ibuprofen. We studied optical separation of racemic Ibuprofen with chiral high performance liquid chromatography (HPLC). Out of three different chiral stationary phases, which were selected on the basis of structure and availability, two were found to be ef-fective. There was optimum eluent composition for each stationary phase for good resolution in optical separation. Resolution decreased with increase of eluent flow rate, but effect of injection volume on resolution was insignificant at high eluent flow rate.
文摘Irbesartan is an antihypertensive drug whose concentration in blood is very small so it requires a sensitive method of analysis, selective and valid for analysis. In this study, it is carried out optimization of analytical conditions and validation for the analysis of irbesartan in plasma. Chromatography was performed on a C 18 column （250 × 4.6 mm, 5 μm） under isocratic elution with acetonitrile-0.1% formic acid （46：54 v/v）, pH 3.75. Detection was made at excitation 250 nm and emission 370 nm and analyses were run at a flow-rate of 1.0 mL/min at a temperature of 40 ℃. Losartan potassium was used as internal standard. Plasma extraction was done by deproteination with acetonitrile, mixed with vortex for 30 seconds, then centrifuged it at 10,000 rpm for 10 rain. In plasma validation, the recovery was 96.22%, and the lower limit of quantification （LLOQ） in plasma was 2 ng/mL. The method also fulfill the criteria for accuracy and precision intra and inter day by normal values （%Diff） not exceed ± 15%. On the stability study, irbesartan in plasma temperature -20 ℃has been stable for 28 days.
