[目的]运用多种表面增强激光解吸-离子化飞行时间质谱(surface-enhanced laser desorption/ionization time of flight mass spectrometry,SELDI-TOF-MS)蛋白质芯片及多元分析方法寻找由乙型肝炎病毒(hepatitis B virus,HBV)感染引起的...[目的]运用多种表面增强激光解吸-离子化飞行时间质谱(surface-enhanced laser desorption/ionization time of flight mass spectrometry,SELDI-TOF-MS)蛋白质芯片及多元分析方法寻找由乙型肝炎病毒(hepatitis B virus,HBV)感染引起的肝纤维化病程相关的血浆生物标志物。[方法]选用多种SELDI化学表面芯片,比较分析肝纤维化病人和正常血浆样本,筛选和确定3种最佳芯片类型。用这3种芯片分析无肝纤维化、轻度肝纤维化、重度肝纤维化和肝硬化4组共110例患者的血浆样本。运用主成分分析(PCA)、偏最小二乘回归(PLSR)、软独立建模分类法(SIMCA)等数据分析技术寻找差异蛋白。用聚类分析法研究差异蛋白的表达相似性。[结果]3种最适芯片类型分别是弱阳离子交换芯片(WCX2)、强阴离子交换芯片(SAX2)、固定化镍金属螯合亲和层析芯片(IMAC-Ni)。这3种芯片吸附的蛋白质种类互不相同,所发现的差异蛋白质峰也不同。经t检验分析,3种芯片共发现了20个差异蛋白峰。运用PCA、PLSR、SIMCA等数据分析技术,分别发现了105、98、62个差异峰,并对差异峰的重要性的可信度进行衡量。运用聚类分析技术,将差异蛋白的表达模式分组。[结论]联用多种SELDI芯片检测,结合多元分析方法,使SELDI技术成为筛选疾病相关的生物学标志物的有力工具。展开更多
Aim To develop an HPLC method with fluorescence detection for the assay ofDL111-IT in rabbit plasma. Methods DL111-IT and internal standard glybenzcyclamide in rabbit plasmawere extracted with chloroform. The determin...Aim To develop an HPLC method with fluorescence detection for the assay ofDL111-IT in rabbit plasma. Methods DL111-IT and internal standard glybenzcyclamide in rabbit plasmawere extracted with chloroform. The determination was performed on a Diamonsil ODS-C_(18) column(150 mm x 4.6 mm, 5 μm) with a mobile phase of acetonitrile and 0.025 mol·L^(-1) diammoniumhydrogen phosphate buffer (pH 5.0, adjusted by phosphoric acid) (60:40, V/V) at a flow-rate of 1.0mL·min^(-1) . Fluorescence detector was operated at excitation wavelength of 250 nm and emissionwavelength of 332 nm. Results The calibration curve in plasma was linear from 1.00 - 20.00ng·mL^(-1) ( r = 0.999 6, n = 5). The method afforded average extracting recoveries of 85.3% ±1.3%, 84.9% ± 2.7% and 85.8% ± 1.8%, and the average method recoveries were 99.5% ±0.4%, 102.1%± 1.8% and 101.3% ± 2.4% for the high (20.00 ng·mL^(-1)) , middle (10.00 ng·mL^(-1)) and low (1.00 ng·mL^(-1)) check samples, respectively. The intra-day (n = 5) and inter-day (n = 5) precisions(RSD) were less than 3.0% and 7.0%, respectively. The limit of detection and quantitation for themethod were 0.3 ng·mL^(-1) (S/N = 3) and 1 ng·mL^(-1) (S/N = 10, RSD<7.0%) plasma sample,respectively. Conclusion The developed method was accurate, sensitive, simple and could be used forpharmacokinetic study of DL111- IT.展开更多
A method for determination of lycopene concentration in dog plasma wasestablished. Methods RP-HPLC was used; the mobile phase consisted of methanol-acetonitrile-methylenechloride (40:30:30, V/V) , the wavelength of de...A method for determination of lycopene concentration in dog plasma wasestablished. Methods RP-HPLC was used; the mobile phase consisted of methanol-acetonitrile-methylenechloride (40:30:30, V/V) , the wavelength of detection was 472 nm, the column temperature wasambient temperature, and the flow rate was 1.0 mL·min^(-1). Results The standard curve was linearin the range from 0.012 4 to 0.496 μg·mL^(-1) with r=0.9992. The average extraction recovery was97.6% +-4.2%. The intra-day and inter-day RSD were 1.52% -4.95% and 2.31% -7.38%, respectively.Conclusion This method is sensitive, rapid, reproducible, and of good selectivity for the analysisof lycopene in dog plasma.展开更多
Artemisinin is a potent anti-malarial drug isolated from traditional Chinese medicinal herb, Artemisia annua. The objective of this study was to develop and validate a sensitive and specific LC-MS/MS method for the de...Artemisinin is a potent anti-malarial drug isolated from traditional Chinese medicinal herb, Artemisia annua. The objective of this study was to develop and validate a sensitive and specific LC-MS/MS method for the determination of artemisinin in rat plasma using amlodipine as Internal Standard. The method consist of a simple liquid-liquid extraction with methyl tertiary butyl ether (MTBE) with subsequent evaporation of the supernatant to dryness followed by the analysis of the reconstituted sample by LC-MS/?vIS with a Z-spray atmospheric pressure ionization (API) interface in the positive ion-multiple reaction monitoring mode to monitor precursor--〉product ions of m/z 282.70--〉m/z 209.0 for artemisinin and m/z 408.9--〉m/z 237.0 for amlodipine respectively. The method was linear (0.999) over the concentration range of 7.8-2000 ng/mL in rat plasma. The intra and inter-day accuracy were measured to be within 94-104.2% and precision (CV) were all less than 5%. The extraction recovery means for internal standard and all the artemisinin concentrations used were between 82-85%.展开更多
Autofluorescence spectra from the serum of health man and cancer patients have been measured and analyzed. Two obviously spectra characteristics of the serum have been discussed in detail. A novel laser cancer diagnos...Autofluorescence spectra from the serum of health man and cancer patients have been measured and analyzed. Two obviously spectra characteristics of the serum have been discussed in detail. A novel laser cancer diagnosis system (LCD-1) has been established and the diagnosis results are compared with clinical methods.展开更多
Carbon black has been widely used in many industrial areas,but it is poor dispersibility in water.In order to improve its dispersibility in water,carbon black was treated by oxygen plasma.Plasma treatment,as one of th...Carbon black has been widely used in many industrial areas,but it is poor dispersibility in water.In order to improve its dispersibility in water,carbon black was treated by oxygen plasma.Plasma treatment,as one of the environmental friendly methods,has been used to introduce polar groups,mainly oxygen-containing groups,to the surface of carbon black.The results show the dispersibility of treated carbon black in water is greatly improved,which is expressed with the centrifugal and gravity settlement rates.Analysis of the treated carbon black with X-ray photoelectron spectroscopy(XPS)indicates that oxygen plasma treatment can cause significant increase of polar groups including C-OH,COOH,CO,and O-C-O on the surface of carbon black thus greatly improves the dispersing stability of carbon black in water.Besides,the dispersibility of plasma treated carbon black can be further improved by the addition of organic amines,especially polyetheramines.The improvement of the dispersing stability of carbon black has also been confirmed by zeta potential measurements.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
文摘[目的]运用多种表面增强激光解吸-离子化飞行时间质谱(surface-enhanced laser desorption/ionization time of flight mass spectrometry,SELDI-TOF-MS)蛋白质芯片及多元分析方法寻找由乙型肝炎病毒(hepatitis B virus,HBV)感染引起的肝纤维化病程相关的血浆生物标志物。[方法]选用多种SELDI化学表面芯片,比较分析肝纤维化病人和正常血浆样本,筛选和确定3种最佳芯片类型。用这3种芯片分析无肝纤维化、轻度肝纤维化、重度肝纤维化和肝硬化4组共110例患者的血浆样本。运用主成分分析(PCA)、偏最小二乘回归(PLSR)、软独立建模分类法(SIMCA)等数据分析技术寻找差异蛋白。用聚类分析法研究差异蛋白的表达相似性。[结果]3种最适芯片类型分别是弱阳离子交换芯片(WCX2)、强阴离子交换芯片(SAX2)、固定化镍金属螯合亲和层析芯片(IMAC-Ni)。这3种芯片吸附的蛋白质种类互不相同,所发现的差异蛋白质峰也不同。经t检验分析,3种芯片共发现了20个差异蛋白峰。运用PCA、PLSR、SIMCA等数据分析技术,分别发现了105、98、62个差异峰,并对差异峰的重要性的可信度进行衡量。运用聚类分析技术,将差异蛋白的表达模式分组。[结论]联用多种SELDI芯片检测,结合多元分析方法,使SELDI技术成为筛选疾病相关的生物学标志物的有力工具。
文摘Aim To develop an HPLC method with fluorescence detection for the assay ofDL111-IT in rabbit plasma. Methods DL111-IT and internal standard glybenzcyclamide in rabbit plasmawere extracted with chloroform. The determination was performed on a Diamonsil ODS-C_(18) column(150 mm x 4.6 mm, 5 μm) with a mobile phase of acetonitrile and 0.025 mol·L^(-1) diammoniumhydrogen phosphate buffer (pH 5.0, adjusted by phosphoric acid) (60:40, V/V) at a flow-rate of 1.0mL·min^(-1) . Fluorescence detector was operated at excitation wavelength of 250 nm and emissionwavelength of 332 nm. Results The calibration curve in plasma was linear from 1.00 - 20.00ng·mL^(-1) ( r = 0.999 6, n = 5). The method afforded average extracting recoveries of 85.3% ±1.3%, 84.9% ± 2.7% and 85.8% ± 1.8%, and the average method recoveries were 99.5% ±0.4%, 102.1%± 1.8% and 101.3% ± 2.4% for the high (20.00 ng·mL^(-1)) , middle (10.00 ng·mL^(-1)) and low (1.00 ng·mL^(-1)) check samples, respectively. The intra-day (n = 5) and inter-day (n = 5) precisions(RSD) were less than 3.0% and 7.0%, respectively. The limit of detection and quantitation for themethod were 0.3 ng·mL^(-1) (S/N = 3) and 1 ng·mL^(-1) (S/N = 10, RSD<7.0%) plasma sample,respectively. Conclusion The developed method was accurate, sensitive, simple and could be used forpharmacokinetic study of DL111- IT.
文摘A method for determination of lycopene concentration in dog plasma wasestablished. Methods RP-HPLC was used; the mobile phase consisted of methanol-acetonitrile-methylenechloride (40:30:30, V/V) , the wavelength of detection was 472 nm, the column temperature wasambient temperature, and the flow rate was 1.0 mL·min^(-1). Results The standard curve was linearin the range from 0.012 4 to 0.496 μg·mL^(-1) with r=0.9992. The average extraction recovery was97.6% +-4.2%. The intra-day and inter-day RSD were 1.52% -4.95% and 2.31% -7.38%, respectively.Conclusion This method is sensitive, rapid, reproducible, and of good selectivity for the analysisof lycopene in dog plasma.
文摘Artemisinin is a potent anti-malarial drug isolated from traditional Chinese medicinal herb, Artemisia annua. The objective of this study was to develop and validate a sensitive and specific LC-MS/MS method for the determination of artemisinin in rat plasma using amlodipine as Internal Standard. The method consist of a simple liquid-liquid extraction with methyl tertiary butyl ether (MTBE) with subsequent evaporation of the supernatant to dryness followed by the analysis of the reconstituted sample by LC-MS/?vIS with a Z-spray atmospheric pressure ionization (API) interface in the positive ion-multiple reaction monitoring mode to monitor precursor--〉product ions of m/z 282.70--〉m/z 209.0 for artemisinin and m/z 408.9--〉m/z 237.0 for amlodipine respectively. The method was linear (0.999) over the concentration range of 7.8-2000 ng/mL in rat plasma. The intra and inter-day accuracy were measured to be within 94-104.2% and precision (CV) were all less than 5%. The extraction recovery means for internal standard and all the artemisinin concentrations used were between 82-85%.
文摘Autofluorescence spectra from the serum of health man and cancer patients have been measured and analyzed. Two obviously spectra characteristics of the serum have been discussed in detail. A novel laser cancer diagnosis system (LCD-1) has been established and the diagnosis results are compared with clinical methods.
基金Program for Changjiang Scholars and Innovative Research Teamin University,China(No.IRT0526)
文摘Carbon black has been widely used in many industrial areas,but it is poor dispersibility in water.In order to improve its dispersibility in water,carbon black was treated by oxygen plasma.Plasma treatment,as one of the environmental friendly methods,has been used to introduce polar groups,mainly oxygen-containing groups,to the surface of carbon black.The results show the dispersibility of treated carbon black in water is greatly improved,which is expressed with the centrifugal and gravity settlement rates.Analysis of the treated carbon black with X-ray photoelectron spectroscopy(XPS)indicates that oxygen plasma treatment can cause significant increase of polar groups including C-OH,COOH,CO,and O-C-O on the surface of carbon black thus greatly improves the dispersing stability of carbon black in water.Besides,the dispersibility of plasma treated carbon black can be further improved by the addition of organic amines,especially polyetheramines.The improvement of the dispersing stability of carbon black has also been confirmed by zeta potential measurements.
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.