The chiral separation of phenylsuccinic acid(PSA)was studied by reversed phase high-performance liquid chromatography(RP-HPLC)with cyclodextrins(CDs)as chiral mobile phase additives.The effects of types of CDs,concent...The chiral separation of phenylsuccinic acid(PSA)was studied by reversed phase high-performance liquid chromatography(RP-HPLC)with cyclodextrins(CDs)as chiral mobile phase additives.The effects of types of CDs,concentration of hydroxypropyl-β-cyclodextrin(HP-β-CD),percentage of organic modifier,pH value and column temperature on enantioselective separation were investigated.The quantification property of the developed RP-HPLC method was examined.The chiral recognition mechanism of PSA was also discussed.The results show that a baseline separation of PSA enantiomers is achieved on a Lichrospher C18 column(4.6 mm(inner diameter)×250 mm,5μm)with HP-β-CD as chiral mobile phase additive.The capacity factors of R-PSA and S-PSA are 3.94 and 4.80,respectively.The separation factor and resolution are respectively 1.22 and 8.03.The mobile phase is a mixture of acetonitrile and deionized water(20-80,volume ratio)containing 10 mmol/L HP-β-CD and 0.05% trifluoroacetic acid(pH 2.5,adjusted with triethylamine)with a flow rate of 1.0 mL/min.The ultraviolet(UV)detector is set at 254 nm.The likely roles are inclusion interaction,induction and hydrogen bonding between HP-β-CD and PSA enantiomers.展开更多
The method of reversed-phase high performance liquid chromatography was established for the determination of effective components in OC-CS spray using double wavelength UV detection.The method was utilized under follo...The method of reversed-phase high performance liquid chromatography was established for the determination of effective components in OC-CS spray using double wavelength UV detection.The method was utilized under following conditions:a column of Kromasil C18(250 mm × 4.6 mm,5 μm),mobile phase consisting of methanol/water(80 /20) at a flow rate of 0.8 mL/min,column temperature of 25 ℃,and the UV detection at 227 nm and 300 nm.Three key components in OC-CS spray could be distinguished clearly,including o-chlorobenzalmalononitrile(CS),oleoresin capsicum(OC) and dihydrocapsaicin(DC).This method has the advantages of fast,simple and satisfactory linear relationship between UV absorption and concentration.It may be considered to turn into a standard method for detection of related components in the spray.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
A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （urid...A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.展开更多
Column packings continue to evolve as the needs of users for high efficiency,high resolution and highly sensitive high performance liquid chromatographic(HPLC) analysis drive further developments.In comparing and cont...Column packings continue to evolve as the needs of users for high efficiency,high resolution and highly sensitive high performance liquid chromatographic(HPLC) analysis drive further developments.In comparing and contrasting modern HPLC columns technologies,diameters of column packings and particle materials are covered.Some products and applications of modern HPLC columns are provided.Future directions in packing developments are predicted in this introductory article.展开更多
Tadalafil(TAD)and dapoxetine HCl(DAP)are recently co-formulated and both show native fluorescence.Therefore,a novel,accurate,specific and sensitive reversed-phase high performance liquid chromatographic method with fl...Tadalafil(TAD)and dapoxetine HCl(DAP)are recently co-formulated and both show native fluorescence.Therefore,a novel,accurate,specific and sensitive reversed-phase high performance liquid chromatographic method with fluorescence detection was developed and validated for their separation and quantitation in dosage form and human plasma using avanafil as an internal standard(IS).Separation was achieved using isocratic elution within 7.0 min on C18column and acetonitrile-0.15%triethylamine(40∶60,v/v;pH 4)as a mobile phase.The flow rate was 1.0 mL/min and the detection was time-programmed at 330,410 and 370 nm for TAD,DAP and IS,respectively,after excitation at 236 nm.The linear ranges from 0.01 to 30.00μg/mL for each drug with the limits of detection of 4.20 and 7.20 ng/mL for TAD and DAP,respectively.The method was validated in accordance to the International Conference on Harmonization(ICH)guidelines and was successfully applied to spiked human plasma with mean recoveries of 98.17%and 98.83%for TAD and DAP respectively.展开更多
Paclitaxel in southern yew tree was quantitatively determined by high performance liquid chromatography (HPLC) with ODS-C18 column. A mixture of CH3OH-H2O-CH3COOH(volume ratio: 55 :44 :1) is used as mobile phase and U...Paclitaxel in southern yew tree was quantitatively determined by high performance liquid chromatography (HPLC) with ODS-C18 column. A mixture of CH3OH-H2O-CH3COOH(volume ratio: 55 :44 :1) is used as mobile phase and UV detection is carried out at 227 nm, and the column temperature is 20℃. The results show that there is a good linear felationship between the area of paclitaxel and the concentration of the sample in the range 50-500 mg/L for paclitaxel. The corresponding regression equation is Y= 13 021. 7 + 1. 01 × 106X, r=0. 9990. The average recovery is 95. 3% and the relative standard deviation is 2. 08%.展开更多
基金Project(20776038)supported by the National Natural Science Foundation of China
文摘The chiral separation of phenylsuccinic acid(PSA)was studied by reversed phase high-performance liquid chromatography(RP-HPLC)with cyclodextrins(CDs)as chiral mobile phase additives.The effects of types of CDs,concentration of hydroxypropyl-β-cyclodextrin(HP-β-CD),percentage of organic modifier,pH value and column temperature on enantioselective separation were investigated.The quantification property of the developed RP-HPLC method was examined.The chiral recognition mechanism of PSA was also discussed.The results show that a baseline separation of PSA enantiomers is achieved on a Lichrospher C18 column(4.6 mm(inner diameter)×250 mm,5μm)with HP-β-CD as chiral mobile phase additive.The capacity factors of R-PSA and S-PSA are 3.94 and 4.80,respectively.The separation factor and resolution are respectively 1.22 and 8.03.The mobile phase is a mixture of acetonitrile and deionized water(20-80,volume ratio)containing 10 mmol/L HP-β-CD and 0.05% trifluoroacetic acid(pH 2.5,adjusted with triethylamine)with a flow rate of 1.0 mL/min.The ultraviolet(UV)detector is set at 254 nm.The likely roles are inclusion interaction,induction and hydrogen bonding between HP-β-CD and PSA enantiomers.
基金Sponsored by the Basic Research Funds of Beijing Institute of Technology (20081642007)
文摘The method of reversed-phase high performance liquid chromatography was established for the determination of effective components in OC-CS spray using double wavelength UV detection.The method was utilized under following conditions:a column of Kromasil C18(250 mm × 4.6 mm,5 μm),mobile phase consisting of methanol/water(80 /20) at a flow rate of 0.8 mL/min,column temperature of 25 ℃,and the UV detection at 227 nm and 300 nm.Three key components in OC-CS spray could be distinguished clearly,including o-chlorobenzalmalononitrile(CS),oleoresin capsicum(OC) and dihydrocapsaicin(DC).This method has the advantages of fast,simple and satisfactory linear relationship between UV absorption and concentration.It may be considered to turn into a standard method for detection of related components in the spray.
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.
文摘A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.
文摘Column packings continue to evolve as the needs of users for high efficiency,high resolution and highly sensitive high performance liquid chromatographic(HPLC) analysis drive further developments.In comparing and contrasting modern HPLC columns technologies,diameters of column packings and particle materials are covered.Some products and applications of modern HPLC columns are provided.Future directions in packing developments are predicted in this introductory article.
文摘Tadalafil(TAD)and dapoxetine HCl(DAP)are recently co-formulated and both show native fluorescence.Therefore,a novel,accurate,specific and sensitive reversed-phase high performance liquid chromatographic method with fluorescence detection was developed and validated for their separation and quantitation in dosage form and human plasma using avanafil as an internal standard(IS).Separation was achieved using isocratic elution within 7.0 min on C18column and acetonitrile-0.15%triethylamine(40∶60,v/v;pH 4)as a mobile phase.The flow rate was 1.0 mL/min and the detection was time-programmed at 330,410 and 370 nm for TAD,DAP and IS,respectively,after excitation at 236 nm.The linear ranges from 0.01 to 30.00μg/mL for each drug with the limits of detection of 4.20 and 7.20 ng/mL for TAD and DAP,respectively.The method was validated in accordance to the International Conference on Harmonization(ICH)guidelines and was successfully applied to spiked human plasma with mean recoveries of 98.17%and 98.83%for TAD and DAP respectively.
基金Project (00KNY1010 ) supported by the Key Program of Science and Technology Office of Hunan Province
文摘Paclitaxel in southern yew tree was quantitatively determined by high performance liquid chromatography (HPLC) with ODS-C18 column. A mixture of CH3OH-H2O-CH3COOH(volume ratio: 55 :44 :1) is used as mobile phase and UV detection is carried out at 227 nm, and the column temperature is 20℃. The results show that there is a good linear felationship between the area of paclitaxel and the concentration of the sample in the range 50-500 mg/L for paclitaxel. The corresponding regression equation is Y= 13 021. 7 + 1. 01 × 106X, r=0. 9990. The average recovery is 95. 3% and the relative standard deviation is 2. 08%.
