Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients a...Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients and 34 healthy volunteers were prepared with this approach. With ultra-performance liquid chromatography（UPLC） coupled with quadrupole time-of-flight mass spectrometry（Q-TOF MS） analysis, the samples were investigated in order to find potential disease biomarkers. After data acquisition, orthogonal signal correction partial least squares models were built to differentiate the healthy volunteers from lung cancer patients and to identify metabolites that showed significantly different expression between the two groups. Several metabolite ions were identified as potential biomarkers according to the variable importance in the project（VIP） value in both ion modes. Five lysophosphatidylcholines were further identified as specifically lysoPC 16：0, isomer of lysoPC 16：0, lysoPC 18：0, lysoPC 18：1 and lysoPC 18：2. These results suggest that UPLC coupled with Q-TOF MS is an effective technique for the analysis of plasma metabolites in metabonomic studies.展开更多
Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism...Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after展开更多
A sensitive analytical method was developed to determine tetrodotoxin（TTX） in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography（UPLC） analysis coupled with tande...A sensitive analytical method was developed to determine tetrodotoxin（TTX） in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography（UPLC） analysis coupled with tandem mass spectrometry（MS/MS） using 11-deoxytetrodotoxin（11-deoxyTTX） as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions（i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX） in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.展开更多
目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高...目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q Exactive Focus MS/MS)法分析制剂的图谱数据,并以Xcalibur 4.0软件拟合分子式,与自建数据库信息进行匹配,初步推测分子式信息,与ChemicalBook或ChemSpider数据库比对,推测化学成分结构。结果共鉴定出158个化学成分,包括苷类36个,黄酮类29个,苯丙素类28个,有机酸类18个,萜类17个,色原酮类8个,其他类22个。结论所建立的方法可系统、准确、快速地定性分析清瘟护肺颗粒中的化学成分。展开更多
建立一种快速测定水产中地西泮的方法。5%氨水乙腈提取,通过EMR固相萃取柱净化,旋蒸浓缩并定容,用内标法对其进行定量。通过超高效液相色谱串联质谱仪测定,使用Agilent ZORBAX Eclipse Plus RRHD C 18柱子分离,流动相乙腈:0.1%甲酸水,...建立一种快速测定水产中地西泮的方法。5%氨水乙腈提取,通过EMR固相萃取柱净化,旋蒸浓缩并定容,用内标法对其进行定量。通过超高效液相色谱串联质谱仪测定,使用Agilent ZORBAX Eclipse Plus RRHD C 18柱子分离,流动相乙腈:0.1%甲酸水,内标法定量,该方法测得的地西泮检出限0.33μg·kg^(-1)和定量限1.1μg·kg^(-1),对样品进行1.10,3.30,11.0μg·kg^(-1)三个梯度加标,平均回收率85.6%~103.3%,精密度为0.8%~3.5%。该研究方法提取简单,回收率和精密度满足要求,可为水产中地西泮残留的检测标准制定提供依据。展开更多
基金Supported by the National Natural Science Foundation of China(No.30801513)the Knowledge Innovation Program of Chinese Academy of Sciences(No.KSCX2-YW-R-170)
文摘Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients and 34 healthy volunteers were prepared with this approach. With ultra-performance liquid chromatography（UPLC） coupled with quadrupole time-of-flight mass spectrometry（Q-TOF MS） analysis, the samples were investigated in order to find potential disease biomarkers. After data acquisition, orthogonal signal correction partial least squares models were built to differentiate the healthy volunteers from lung cancer patients and to identify metabolites that showed significantly different expression between the two groups. Several metabolite ions were identified as potential biomarkers according to the variable importance in the project（VIP） value in both ion modes. Five lysophosphatidylcholines were further identified as specifically lysoPC 16：0, isomer of lysoPC 16：0, lysoPC 18：0, lysoPC 18：1 and lysoPC 18：2. These results suggest that UPLC coupled with Q-TOF MS is an effective technique for the analysis of plasma metabolites in metabonomic studies.
基金partly supported by National Natural Science Foundation of China(No.81430095)also by Special National Program on Key Basic Research Project(No.2014CB560706)
文摘Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after
基金Supported by the National Key Research and Development Program of China(No.2016YFF0201104)the Construction of Public Service Platform for Research and Test of Marine Pilot Technology of China(No.Bhsfs009)the Project of Xiamen Southern oceanographic Center,China(No.16PFW008SF15).
文摘A sensitive analytical method was developed to determine tetrodotoxin（TTX） in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography（UPLC） analysis coupled with tandem mass spectrometry（MS/MS） using 11-deoxytetrodotoxin（11-deoxyTTX） as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions（i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX） in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples.
文摘建立一种快速测定水产中地西泮的方法。5%氨水乙腈提取,通过EMR固相萃取柱净化,旋蒸浓缩并定容,用内标法对其进行定量。通过超高效液相色谱串联质谱仪测定,使用Agilent ZORBAX Eclipse Plus RRHD C 18柱子分离,流动相乙腈:0.1%甲酸水,内标法定量,该方法测得的地西泮检出限0.33μg·kg^(-1)和定量限1.1μg·kg^(-1),对样品进行1.10,3.30,11.0μg·kg^(-1)三个梯度加标,平均回收率85.6%~103.3%,精密度为0.8%~3.5%。该研究方法提取简单,回收率和精密度满足要求,可为水产中地西泮残留的检测标准制定提供依据。
