ABSTRACT A quantitative method for the assay of free cholesterol has been described in this paper. The experimental conditions for the determination of cholesterol in serum by Thin-layer chromatography were disscused....ABSTRACT A quantitative method for the assay of free cholesterol has been described in this paper. The experimental conditions for the determination of cholesterol in serum by Thin-layer chromatography were disscused. The solvent System was petroleum ether-ethyl acetate-glacial acetic acid (8o:20:1) and the spra-ying reagent was a solution of sulphuric acid and vanillin. Under the selected con-ditions, the peak area was linearly related to the cholesterol amount for the range between 80～700 ng per spot. The intraplate and interplate coefficients were 2.4% and 7.4% respectively. The recovery of cholesterol was 101.6%. The method presented was simple, rapid and accurate. The results of experi-mental investigation and clinical application were satisfactory.展开更多
The separation of Co 2+ from Zn 2+ , Cd 2+ by anion exchange chromatography was discussed. The chromatographic column containing anion resin 201×7 which was saturated with a solution of ammonium chloride. The eff...The separation of Co 2+ from Zn 2+ , Cd 2+ by anion exchange chromatography was discussed. The chromatographic column containing anion resin 201×7 which was saturated with a solution of ammonium chloride. The effects of the eluant acidity and eluant composition on the separation were investigated. The results indicate that this anion exchange chromatography is suitable to the separation of Co 2+ from Zn 2+ , Cd 2+ , and the condition of separation is simple and convenient. When the column is saturated with NH 4Cl solution (2.0 mol/L, pH=4.0), the separation can be completed effectively. Zn 2+ and Cd 2+ can also be separa ted when different eluants are used and the pure solution with high concentration of Zn 2+ , Cd 2+ respectively can be obtained ea sily.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 method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, ...A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.展开更多
Chiral ionic liquids (CILs) containing imidazolium cations and L-Proline (L-Pro) anions were applied as chiral selector to separate tryptophan (Trp) enantiomers on a C18 column by ligand exchange chromatography. Sever...Chiral ionic liquids (CILs) containing imidazolium cations and L-Proline (L-Pro) anions were applied as chiral selector to separate tryptophan (Trp) enantiomers on a C18 column by ligand exchange chromatography. Several factors influencing Trp enantiomers separation, such as alkyl chain length of CILs, concentrations of Cu2+ and CILs, pH of the mobile phase, flow rate, organic solvent and temperature, were studied. Under the optimal conditions, the Trp enantiomers could be successfully separated within 21 min with the resolution of 2.30. At the same time, some thermodynamical parameters were obtained. The experimental results show that the enthalpy values of the Trp enantiomers are negative, indicating that the separation process is exothermic. And the enthalpy values of D-Trp are larger than those of L-Trp, which indicates that L-Trp could form more stable ternary complexes with tryptophan enantiomers.展开更多
Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation ...Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.展开更多
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
A high-performance liquid chromatography was describ-ed to measure the concentration of human 3-methylhistidine in urine witho-phthaldialdehyde pre-column derivatization.This assay system resultedin a clear separation...A high-performance liquid chromatography was describ-ed to measure the concentration of human 3-methylhistidine in urine witho-phthaldialdehyde pre-column derivatization.This assay system resultedin a clear separation of 3-methylhistidine derivative from other derivativ-es in urine within 25 min.Linearity,recovery and coefficients of vari-ation were studied.The method has been successfully applied to routineanalysis for clinical studies and diagnosis.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
A gas chromatographic method for determining the trace residue of imazethapyr {(±)-2-[4,5-dihydro-4-methtyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl]-5-ehtyl-3-pyridinecarboxylic acid} in soil was described in th...A gas chromatographic method for determining the trace residue of imazethapyr {(±)-2-[4,5-dihydro-4-methtyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl]-5-ehtyl-3-pyridinecarboxylic acid} in soil was described in this paper. The soil samples were extracted by shaking with 0.5 mol·L -1 sodium hydroxide solution. The aqueous extract was acidified with hydrocholric acid to adjust the pH to 2.0 to precipitate humic acids, then was extracted with dichloromethane. The organic extract was dried with anhydrous sodium sulfate and was concentrated. After florisil cleanup, and imazethapyr is derivatized with trimethylanilinium hydroxide (TMAH). Methylated imazethapyr was analyzed by gas chromatography with a nitrogen-phosphorous dtector. The recovery of imazethapyr from soil samples are over 80%, the experimental detection limit of the method is 5ng·g -1 .展开更多
A method was developed for the simultaneous determination of four kinds of estrogens （hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol） in feed by gas chromatography-mass spectrometry （GC-MS）. After ...A method was developed for the simultaneous determination of four kinds of estrogens （hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol） in feed by gas chromatography-mass spectrometry （GC-MS）. After the sample was extracted by ethyl ether and cleaned-up on HLB phase extraction column, four kinds of estrogens were derived and quantified in gas chromatographymass spectrometry. The results showed that the linear detectable ranged from 2.5 ng· mL-1 to 250 ng· mL-1for hexoestrol and from 5 ng· mL-1 to 500 ng· mL-1 for three other estrogens with the correlation coefficients （R2） were no less than 0.990. The recoveries were in the range of 76.34%-96.33% and the relative standard deviation was no more than 22.7%. The limits of quantitation （LOQ） for all analytics were between 10 ug· kg^-1 and 20 ug· kg^-1. The method was accurate and sensitive and could meet the actual requirements for the analyses of feed samples.展开更多
The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tande...The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines.展开更多
Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC...Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine.展开更多
Steroids comprise a large group of natural substances that must frequently be monitored in various biological materials. Due to the metabolic versatility of steroid molecules, extremely complex mixtures are often enco...Steroids comprise a large group of natural substances that must frequently be monitored in various biological materials. Due to the metabolic versatility of steroid molecules, extremely complex mixtures are often encountered, necessitating the use of a chromatographic procedure prior to measurement. In this article we present our work, that is, the development of analyses of biological steroids (especially vitamin D compounds and neurosteroids) using gas chromatography/mass spectrometry, high-performance liquid chromatography (including inclusion chromatography using cyclodextrin) and liquid chromatography/mass spectrometry.展开更多
A review on the principles and applications of boronic acids as affinity ligands for the chromatographic separation of carbohydrates,nucleic acid components,glycoproteins,and other small biomolecules.The mechanisms of...A review on the principles and applications of boronic acids as affinity ligands for the chromatographic separation of carbohydrates,nucleic acid components,glycoproteins,and other small biomolecules.The mechanisms of interactions between boronate ligands and analytes are described.Various boronate ligands and supports are discussed.Examples of the use of boronate affinity chromatography for separation of each class of analytes are presented.展开更多
L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum （ATCC 21799） strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography....L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum （ATCC 21799） strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 （g/（g·h）） （per gram resin and per hour） at an eluent flow rate of 10 （mL/min） in fixed-bed chromatography. The results obtained from SMB were 0.11 （g/（g·h）） for L-lysine purification rate and 96% for L-lysine recovery.展开更多
Laboratory generated spent bleached liquor from the chlorination, caustic extraction stage of mixed wood kraft pulp processing has been analyzed both qualitatively and quantitatively for various resin & fatty acid...Laboratory generated spent bleached liquor from the chlorination, caustic extraction stage of mixed wood kraft pulp processing has been analyzed both qualitatively and quantitatively for various resin & fatty acids by using GC. A number of resin acids, saturated and unsaturated fatty acids, chloro fatty and resin acid have been detected and their concentrations are estimated. The results are compared with results on different agriculture residue/hardwood pulps, which were reported earlier. The concentrations of various compounds detected have also been compared with their reported LC50 values.展开更多
文摘ABSTRACT A quantitative method for the assay of free cholesterol has been described in this paper. The experimental conditions for the determination of cholesterol in serum by Thin-layer chromatography were disscused. The solvent System was petroleum ether-ethyl acetate-glacial acetic acid (8o:20:1) and the spra-ying reagent was a solution of sulphuric acid and vanillin. Under the selected con-ditions, the peak area was linearly related to the cholesterol amount for the range between 80～700 ng per spot. The intraplate and interplate coefficients were 2.4% and 7.4% respectively. The recovery of cholesterol was 101.6%. The method presented was simple, rapid and accurate. The results of experi-mental investigation and clinical application were satisfactory.
文摘The separation of Co 2+ from Zn 2+ , Cd 2+ by anion exchange chromatography was discussed. The chromatographic column containing anion resin 201×7 which was saturated with a solution of ammonium chloride. The effects of the eluant acidity and eluant composition on the separation were investigated. The results indicate that this anion exchange chromatography is suitable to the separation of Co 2+ from Zn 2+ , Cd 2+ , and the condition of separation is simple and convenient. When the column is saturated with NH 4Cl solution (2.0 mol/L, pH=4.0), the separation can be completed effectively. Zn 2+ and Cd 2+ can also be separa ted when different eluants are used and the pure solution with high concentration of Zn 2+ , Cd 2+ respectively can be obtained ea sily.
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(2005CB623702) supported by the National Key Basic Research Program of China
文摘A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.
基金Project(21176262) supported by the National Natural Science Foundation of ChinaProject(2010WK3029) supported by Science and Technology Program of Hunan Province,China
文摘Chiral ionic liquids (CILs) containing imidazolium cations and L-Proline (L-Pro) anions were applied as chiral selector to separate tryptophan (Trp) enantiomers on a C18 column by ligand exchange chromatography. Several factors influencing Trp enantiomers separation, such as alkyl chain length of CILs, concentrations of Cu2+ and CILs, pH of the mobile phase, flow rate, organic solvent and temperature, were studied. Under the optimal conditions, the Trp enantiomers could be successfully separated within 21 min with the resolution of 2.30. At the same time, some thermodynamical parameters were obtained. The experimental results show that the enthalpy values of the Trp enantiomers are negative, indicating that the separation process is exothermic. And the enthalpy values of D-Trp are larger than those of L-Trp, which indicates that L-Trp could form more stable ternary complexes with tryptophan enantiomers.
文摘Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.
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.
文摘A high-performance liquid chromatography was describ-ed to measure the concentration of human 3-methylhistidine in urine witho-phthaldialdehyde pre-column derivatization.This assay system resultedin a clear separation of 3-methylhistidine derivative from other derivativ-es in urine within 25 min.Linearity,recovery and coefficients of vari-ation were studied.The method has been successfully applied to routineanalysis for clinical studies and diagnosis.
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.
文摘A gas chromatographic method for determining the trace residue of imazethapyr {(±)-2-[4,5-dihydro-4-methtyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl]-5-ehtyl-3-pyridinecarboxylic acid} in soil was described in this paper. The soil samples were extracted by shaking with 0.5 mol·L -1 sodium hydroxide solution. The aqueous extract was acidified with hydrocholric acid to adjust the pH to 2.0 to precipitate humic acids, then was extracted with dichloromethane. The organic extract was dried with anhydrous sodium sulfate and was concentrated. After florisil cleanup, and imazethapyr is derivatized with trimethylanilinium hydroxide (TMAH). Methylated imazethapyr was analyzed by gas chromatography with a nitrogen-phosphorous dtector. The recovery of imazethapyr from soil samples are over 80%, the experimental detection limit of the method is 5ng·g -1 .
基金Supported by Fund of Harbin Provincial Education Department(2014AB3BN041)
文摘A method was developed for the simultaneous determination of four kinds of estrogens （hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol） in feed by gas chromatography-mass spectrometry （GC-MS）. After the sample was extracted by ethyl ether and cleaned-up on HLB phase extraction column, four kinds of estrogens were derived and quantified in gas chromatographymass spectrometry. The results showed that the linear detectable ranged from 2.5 ng· mL-1 to 250 ng· mL-1for hexoestrol and from 5 ng· mL-1 to 500 ng· mL-1 for three other estrogens with the correlation coefficients （R2） were no less than 0.990. The recoveries were in the range of 76.34%-96.33% and the relative standard deviation was no more than 22.7%. The limits of quantitation （LOQ） for all analytics were between 10 ug· kg^-1 and 20 ug· kg^-1. The method was accurate and sensitive and could meet the actual requirements for the analyses of feed samples.
文摘The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines.
文摘Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine.
基金Grants from the Ministry of Education,Science,Sports and Culture of Japan
文摘Steroids comprise a large group of natural substances that must frequently be monitored in various biological materials. Due to the metabolic versatility of steroid molecules, extremely complex mixtures are often encountered, necessitating the use of a chromatographic procedure prior to measurement. In this article we present our work, that is, the development of analyses of biological steroids (especially vitamin D compounds and neurosteroids) using gas chromatography/mass spectrometry, high-performance liquid chromatography (including inclusion chromatography using cyclodextrin) and liquid chromatography/mass spectrometry.
文摘A review on the principles and applications of boronic acids as affinity ligands for the chromatographic separation of carbohydrates,nucleic acid components,glycoproteins,and other small biomolecules.The mechanisms of interactions between boronate ligands and analytes are described.Various boronate ligands and supports are discussed.Examples of the use of boronate affinity chromatography for separation of each class of analytes are presented.
基金Grant in AidforScientificResearchfromTheJapanSocietyforthePromotionofScience(JSPS) ,Grant in AidforYoungScientistsfromTheMinistryofEducation ,Culture ,Sports ,ScienceandTechnology (MEXT)
文摘L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum （ATCC 21799） strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 （g/（g·h）） （per gram resin and per hour） at an eluent flow rate of 10 （mL/min） in fixed-bed chromatography. The results obtained from SMB were 0.11 （g/（g·h）） for L-lysine purification rate and 96% for L-lysine recovery.
文摘Laboratory generated spent bleached liquor from the chlorination, caustic extraction stage of mixed wood kraft pulp processing has been analyzed both qualitatively and quantitatively for various resin & fatty acids by using GC. A number of resin acids, saturated and unsaturated fatty acids, chloro fatty and resin acid have been detected and their concentrations are estimated. The results are compared with results on different agriculture residue/hardwood pulps, which were reported earlier. The concentrations of various compounds detected have also been compared with their reported LC50 values.
