The determination method of 10-hydroxycamptothecin in Camptotheca acuminata fruits by high-performance liquid chromatogram (HPLC) was studied. The HPLC analysis was performed on a HIQ sil C18(4.6×250 mm) column w...The determination method of 10-hydroxycamptothecin in Camptotheca acuminata fruits by high-performance liquid chromatogram (HPLC) was studied. The HPLC analysis was performed on a HIQ sil C18(4.6×250 mm) column with mobile phase of acetonitrilewater (3:7, V:V), flow rate 1 mLmin-1 and UV detective wavelength 266 nm. Extracting 10-hydroxycamptothecin by ultrasonic method from fruits of C. acuminata to prepare samples for analysis was systematically discussed. The optimal extraction condition was carried out by 60% alcohol solution at 60℃ for 50 minutes.展开更多
The aim of the study is to investigate the contents of trace element Se, Cd, Pb in three plants including burdock, ginkgol and garlic via graphite furnace atomic absorption and standard addition method. The results sh...The aim of the study is to investigate the contents of trace element Se, Cd, Pb in three plants including burdock, ginkgol and garlic via graphite furnace atomic absorption and standard addition method. The results show that Se in burdock stem, skin and leaf are 32.40, 48.63, 38.10 μg/g, respectively; Cd in burdock stem, skin and leaf are 0. 160 0, 0. 300 0, 0. 140 0 μg/g, respectively; Cd in burdock stem, skin and leaf are 2. 020, 3. 960, 2. 410 μg/g, respectively. In the ginkgo and ginko leaf, Se contents are 17.63 and 16.91 μg/g, respectively ; for Cd are 0. 181 0 and 0.2020μg/g, respectively ; for Pb are 3. 572 and 4. 021 μg/g, respectively. In garlic, Se, Cd and Pb are 73. 900 0, 6. 900 0 and 0. 390 0, respectively. All the standard deviations of measured results are below 2.3%, recovery rate are from 99% to 101%.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
A rapid, accurate and sensitive HPLC method for the determination of bupropion hydrochloride in a new tablet formulation is described. Chromatographic separation of bupropion hydrochloride is achieved using a mobile p...A rapid, accurate and sensitive HPLC method for the determination of bupropion hydrochloride in a new tablet formulation is described. Chromatographic separation of bupropion hydrochloride is achieved using a mobile phase consisting of methanol -0.01 mol·L -1 ammonium dihydrogen phosphate (80:20, v/v, pH 4.8) at a flow rate of 1.0 mL·min -1 on a Hypersil BDS C18 column. Absorbance is monitored at 251 nm where bupropion hydrochloride has maximum absorption in the mobile phase. The linear range of determination for bupropion hydrochloride is between 2.12 and 21.2 μg·mL -1. The proposed method was validated with respect to accuracy, precision, limits of detection and quantification and robustness, etc.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
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
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.
Using the glucose and L-glutamic-acid to prepare the standard substance according to the ratio of 1：1, and the artificial seawater and the standard substance to prepare a series of standard solutions, the distributio...Using the glucose and L-glutamic-acid to prepare the standard substance according to the ratio of 1：1, and the artificial seawater and the standard substance to prepare a series of standard solutions, the distribution pattern of uncertainty in measurement of seawater COD is obtained based on the measured results of the series of standard solutions by the potassium iodide-alkaline potassium permanganate determination method. The distribution pattern is as follows： Uncertainty in measurement is big and not constant at the high end, but small and constant at the low end.展开更多
[Objective] This study aimed to establish a method for quantitative detection of mRNA transcriptional level of SS2 adhesive related-factors of Streptococcus suis serotype 2 （SS2） by fluorescent quantitative PCR. []V...[Objective] This study aimed to establish a method for quantitative detection of mRNA transcriptional level of SS2 adhesive related-factors of Streptococcus suis serotype 2 （SS2） by fluorescent quantitative PCR. []Vlethod] The gene fragments en- coding SS2 adhesive related-factors MRP, FBPS and CPS2J and a housekeeping gene aroA were amplified by reverse transcription PCR from the total RNA of SS2, cloned, and sequenced. The recombinant plasmids containing the target genes were constructed, and used as templates in Real-time PCR. [Result] Dynamic curves, stan- dard curves and melting curves of the adhesive related-factors and aroA were ob- tained by the optimized Real-time PCR system. The standard curves showed a good linear relationship between template copy number and circulation number, and the correlation coefficients （FF） of the standard curves were over 0.995. Also, these as- says were highly specific a^d there was single specific melting peak for every gene. Moreover, the assays were highly sensitive and had a detection limit of 1.0×102 copies in 1 μl of initial templates. Finally, it was highly repeatable and had a coeffi- cient of variation less than 2% for intra-assay. [Conclusion] This study will provide a way to reveal the adhesion mechanism of SS2 to different host cells at molecular level.展开更多
This paper describes an effective method for determining chlordiazepoxide. An excess of sodium tetraphenylboron is added to precipitate chlordiazepoxide in HAc NaAc buffer solution (pH=4.0). After filtering off the p...This paper describes an effective method for determining chlordiazepoxide. An excess of sodium tetraphenylboron is added to precipitate chlordiazepoxide in HAc NaAc buffer solution (pH=4.0). After filtering off the precipitate, the excessive sodium tetraphenylboron in the filtrate is titrated with cetyltrimethylammonium bromide standard solution, with bromophenol blue as indicator. The method is simple and rapid, it has been applied for the determination of chlordiazepoxide raw materials with satisfactory results. The recovery is between 99.58% and 100.4%, the relative error is less than ± 0.50% . Experiments show that the method gives the same results as the approach using nonaqueous titration (ChP).展开更多
A reversed-phase high performance liquid chromatographic (RP-HPLC) method wasdeveloped and validated for the simultaneous deteimination of ceftazidime and tazobactam ininject-able powder. Methods Chromatography was ca...A reversed-phase high performance liquid chromatographic (RP-HPLC) method wasdeveloped and validated for the simultaneous deteimination of ceftazidime and tazobactam ininject-able powder. Methods Chromatography was carried out on Zorbax 300SB-C_(18) column using amixture of methanol and aqueous solution of phosphate buffer (pH = 5.6) as mobile phase. The UVdetection wavelength was 220 run. Results The linear ranges of ceftazidime and tazobactam were 0.62- 631.8 μg·mL^(-1) and 0.66 - 677.50 μg·mL^(-1), respectively. The average recoveries were 98.8%- 101.4% for ceftazidime, and 99,1% - 100.2% for tazobactam. The RSD values of inter-day andintra-day assays were lower than 1.5% for ceftazidime and 2.6% for tazobactam. Conclusion Thismethod is reproducible, simple, precise, and rapid for the quality control of ceftazidime andtazobactam in injectable powder.展开更多
基金This paper was supported by National Natural Science Foundation of China (No. 30070086).
文摘The determination method of 10-hydroxycamptothecin in Camptotheca acuminata fruits by high-performance liquid chromatogram (HPLC) was studied. The HPLC analysis was performed on a HIQ sil C18(4.6×250 mm) column with mobile phase of acetonitrilewater (3:7, V:V), flow rate 1 mLmin-1 and UV detective wavelength 266 nm. Extracting 10-hydroxycamptothecin by ultrasonic method from fruits of C. acuminata to prepare samples for analysis was systematically discussed. The optimal extraction condition was carried out by 60% alcohol solution at 60℃ for 50 minutes.
基金School Fund of Xuzhou Institute of Technology (XKY200614)~~
文摘The aim of the study is to investigate the contents of trace element Se, Cd, Pb in three plants including burdock, ginkgol and garlic via graphite furnace atomic absorption and standard addition method. The results show that Se in burdock stem, skin and leaf are 32.40, 48.63, 38.10 μg/g, respectively; Cd in burdock stem, skin and leaf are 0. 160 0, 0. 300 0, 0. 140 0 μg/g, respectively; Cd in burdock stem, skin and leaf are 2. 020, 3. 960, 2. 410 μg/g, respectively. In the ginkgo and ginko leaf, Se contents are 17.63 and 16.91 μg/g, respectively ; for Cd are 0. 181 0 and 0.2020μg/g, respectively ; for Pb are 3. 572 and 4. 021 μg/g, respectively. In garlic, Se, Cd and Pb are 73. 900 0, 6. 900 0 and 0. 390 0, respectively. All the standard deviations of measured results are below 2.3%, recovery rate are from 99% to 101%.
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A rapid, accurate and sensitive HPLC method for the determination of bupropion hydrochloride in a new tablet formulation is described. Chromatographic separation of bupropion hydrochloride is achieved using a mobile phase consisting of methanol -0.01 mol·L -1 ammonium dihydrogen phosphate (80:20, v/v, pH 4.8) at a flow rate of 1.0 mL·min -1 on a Hypersil BDS C18 column. Absorbance is monitored at 251 nm where bupropion hydrochloride has maximum absorption in the mobile phase. The linear range of determination for bupropion hydrochloride is between 2.12 and 21.2 μg·mL -1. The proposed method was validated with respect to accuracy, precision, limits of detection and quantification and robustness, etc.
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.
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Using the glucose and L-glutamic-acid to prepare the standard substance according to the ratio of 1：1, and the artificial seawater and the standard substance to prepare a series of standard solutions, the distribution pattern of uncertainty in measurement of seawater COD is obtained based on the measured results of the series of standard solutions by the potassium iodide-alkaline potassium permanganate determination method. The distribution pattern is as follows： Uncertainty in measurement is big and not constant at the high end, but small and constant at the low end.
基金Supported by National Natural Science Foundation of China(31072155)Natural Science Foundation of Jiangsu Province(BK2010068)+1 种基金Fund for Independent Innovation of Agricultural Science in Jiangsu Province[CX(11)2060]Special Fund for Agroscientific Research in the Public Interest(201303041)~~
文摘[Objective] This study aimed to establish a method for quantitative detection of mRNA transcriptional level of SS2 adhesive related-factors of Streptococcus suis serotype 2 （SS2） by fluorescent quantitative PCR. []Vlethod] The gene fragments en- coding SS2 adhesive related-factors MRP, FBPS and CPS2J and a housekeeping gene aroA were amplified by reverse transcription PCR from the total RNA of SS2, cloned, and sequenced. The recombinant plasmids containing the target genes were constructed, and used as templates in Real-time PCR. [Result] Dynamic curves, stan- dard curves and melting curves of the adhesive related-factors and aroA were ob- tained by the optimized Real-time PCR system. The standard curves showed a good linear relationship between template copy number and circulation number, and the correlation coefficients （FF） of the standard curves were over 0.995. Also, these as- says were highly specific a^d there was single specific melting peak for every gene. Moreover, the assays were highly sensitive and had a detection limit of 1.0×102 copies in 1 μl of initial templates. Finally, it was highly repeatable and had a coeffi- cient of variation less than 2% for intra-assay. [Conclusion] This study will provide a way to reveal the adhesion mechanism of SS2 to different host cells at molecular level.
文摘This paper describes an effective method for determining chlordiazepoxide. An excess of sodium tetraphenylboron is added to precipitate chlordiazepoxide in HAc NaAc buffer solution (pH=4.0). After filtering off the precipitate, the excessive sodium tetraphenylboron in the filtrate is titrated with cetyltrimethylammonium bromide standard solution, with bromophenol blue as indicator. The method is simple and rapid, it has been applied for the determination of chlordiazepoxide raw materials with satisfactory results. The recovery is between 99.58% and 100.4%, the relative error is less than ± 0.50% . Experiments show that the method gives the same results as the approach using nonaqueous titration (ChP).
文摘A reversed-phase high performance liquid chromatographic (RP-HPLC) method wasdeveloped and validated for the simultaneous deteimination of ceftazidime and tazobactam ininject-able powder. Methods Chromatography was carried out on Zorbax 300SB-C_(18) column using amixture of methanol and aqueous solution of phosphate buffer (pH = 5.6) as mobile phase. The UVdetection wavelength was 220 run. Results The linear ranges of ceftazidime and tazobactam were 0.62- 631.8 μg·mL^(-1) and 0.66 - 677.50 μg·mL^(-1), respectively. The average recoveries were 98.8%- 101.4% for ceftazidime, and 99,1% - 100.2% for tazobactam. The RSD values of inter-day andintra-day assays were lower than 1.5% for ceftazidime and 2.6% for tazobactam. Conclusion Thismethod is reproducible, simple, precise, and rapid for the quality control of ceftazidime andtazobactam in injectable powder.
