Biological mass spectrometry has received a great progress in recent years.The osteopontin(OPN) isolated and purified from the human milk was studied by HPLC using SCX and C4 columns.After hydrolyzing the purified OPN...Biological mass spectrometry has received a great progress in recent years.The osteopontin(OPN) isolated and purified from the human milk was studied by HPLC using SCX and C4 columns.After hydrolyzing the purified OPN sample by trypsin,the correlative polypeptide fragments GDSVVYGLR and QNLLAPQTLPSK were obtained by FT-ICR-MS.It showed that the method of nano-spray HPLC combined with FT-ICR-MS and Mascot search was very efficient for the analysis of the purified OPN and its polypeptide fragments.Further study provides more academic theories of their different modifications and the relative bioactivities.展开更多
FT-ICR-MS technology has significant sensitivity and dynamic range,enabling the detection of different fragmentations of peptides and proteins at lower and lower levels.In the bottom-up approach,by far the most freque...FT-ICR-MS technology has significant sensitivity and dynamic range,enabling the detection of different fragmentations of peptides and proteins at lower and lower levels.In the bottom-up approach,by far the most frequently used proteomics approach,a single LC-MS run can reveal tens and even hundreds of useful information.For each peptide selected for MS/MS,two data-files were generated,one for ECD and another one for CAD.They were merged as described and submitted to the Mascot search engine using the protein database.These thresholds ensure almost 100% statistical confident in the peptide identification.展开更多
The phosphorothioate oligonucleotides are used more and more for cancer treatment.Fast analysis of phosphorothioate oligonucleotide is important for quality control of this drug.In this paper,FT-ICR-MS was used to ana...The phosphorothioate oligonucleotides are used more and more for cancer treatment.Fast analysis of phosphorothioate oligonucleotide is important for quality control of this drug.In this paper,FT-ICR-MS was used to analyze a phosphorothioate oligonucleotide with 6 321 u.Experimental results showed that accurate relative molecular mass of phosphorothioate oligonucleotide determined by FT-ICR-MS can be used for confirmation of its composition.展开更多
目的采用高效液相色谱串联高分辨傅立叶变换离子回旋共振质谱(High performance liquid chromatography tandem high resolution Fourier transform ion cyclotron resonance mass spectrometry,HPLC-FTICR-MS)技术对芪红水煎剂的化学...目的采用高效液相色谱串联高分辨傅立叶变换离子回旋共振质谱(High performance liquid chromatography tandem high resolution Fourier transform ion cyclotron resonance mass spectrometry,HPLC-FTICR-MS)技术对芪红水煎剂的化学成分进行快速表征,建立高效液相色谱法(high-performance liquid chromatography,HPLC)对芪红水煎剂中多成分进行含量测定,分析黄芪、水红花子配伍对主要成分溶出的影响,完善其质量控制。方法HPLC-FT-ICR-MS采用电喷雾离子化源(Electrospray ionization source,ESI)负离子模式检测,根据高分辨数据及二级质谱信息结合对照品数据及相关文献对芪红水煎剂化学成分进行快速鉴定;芪红水煎剂中6种主要成分的HPLC含量测定采用Venusil MP-C18色谱柱(4.6 mm×250 mm,5μm),甲醇-0.5%磷酸溶液梯度洗脱,流速1.0 mL·min^-1,检测波长254 nm和290 nm。结果对芪红水煎剂提取物中的26个化学成分进行表征,其中9个成分来源于水红花子,17个成分来源于黄芪。与单味药相比,芪红水煎剂中毛蕊异黄酮-7-O-β-D-葡萄糖苷、N-反式-阿魏酰酪胺、槲皮素的煎出量均明显增加(P<0.01),花旗松素、芒柄花素的煎出量明显降低(P<0.01),毛蕊异黄酮煎出量变化不明显(P>0.05)。结论该方法可快速对芪红水煎剂中的主要成分进行定性分析,所建多成分含量测定方法可以反映水红花子和黄芪共煎后对主要成分溶出率的影响,为进一步研究其配伍规律提供理论依据。展开更多
Milk as a key element for infant nutrition represents the only source of feeding for newborns and infants, breast-feeding milk normally contains several bioactive proteins or peptides useful for the development of the...Milk as a key element for infant nutrition represents the only source of feeding for newborns and infants, breast-feeding milk normally contains several bioactive proteins or peptides useful for the development of the immune system that protects infants from diseases. Osteopontin（OPN） plays a distinct role during the processes of lactation, Some studies on OPN isolated and purified from the human milk via HPLC on SCX and Ca columns adopted biological mass spectrometry. After digesting the purified OPN sample with trypsin, the typical correlative polypeptide fragments GDSVVYGLR and QNLLAPQTLPSK are identified by FT-ICR-MS. The rapid identification of OPN is assumed to be reasonably well behaving in a standard bottom-up experiment. It shows that nano-spray HPLC combined with FT-ICR-MS and Mascot search can be used as a high efficient method for the identification of purified OPN and its polypeptide fragments. Further study will provide more academic theories of their different modifications and the bioactivity as well.展开更多
The coupling of capillary electrophoresis to electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) was presented for the on-line separation and detection of mixture of peptides. With th...The coupling of capillary electrophoresis to electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) was presented for the on-line separation and detection of mixture of peptides. With the ultra-high resolution and unmatchable mass measurement accuracy FT-ICR-MS provides, the separation and identification of angiotensin III, octreotide and elastin chemotactic were successfully achieved using this fabricated device, which showed its great application potential in detection and structural identification for multicomponent sample.展开更多
为了认识稠油开发过程中低温氧化与高温氧化阶段原油变化规律,利用静态氧化釜开展稠油的高低温氧化实验,借助傅里叶变换离子回旋共振质谱分析技术对高低温氧化前后的原油分子量及O、N、S杂原子化合物特征开展研究,结果表明:原油低温氧...为了认识稠油开发过程中低温氧化与高温氧化阶段原油变化规律,利用静态氧化釜开展稠油的高低温氧化实验,借助傅里叶变换离子回旋共振质谱分析技术对高低温氧化前后的原油分子量及O、N、S杂原子化合物特征开展研究,结果表明:原油低温氧化阶段分子量分布特征与原样相似,相对分子量分布范围在200~750,整体呈平缓状单峰型分布,高温氧化阶段分子量分布范围前移,呈明显的前峰单峰型分布;杂原子化合物中的O元素在低温氧化阶段主要以无环的饱和二元酸形式存在,在高温氧化阶段受环化、芳构化及脱甲基作用的影响,伴随着侧链烷基及杂原子基团的断裂和芳构化过程,造成原油中杂原子化合物向着碳数更小、双键当量(double bond equivalents,DBE)值更低的方向演化。该研究探索了温度与原油结构及化学组成之间的关系,对于指导稠油开发现场具有重要意义。展开更多
溶解性有机碳(Dissolved organic carbon,DOC)是农田土壤碳库中最重要的活性碳组分。DOC可为土壤微生物提供必需的营养元素,也会诱导复杂的环境效应。本研究以中国青岛市大沽河农业区为研究对象,利用室内培养实验,并结合傅里叶变换离子...溶解性有机碳(Dissolved organic carbon,DOC)是农田土壤碳库中最重要的活性碳组分。DOC可为土壤微生物提供必需的营养元素,也会诱导复杂的环境效应。本研究以中国青岛市大沽河农业区为研究对象,利用室内培养实验,并结合傅里叶变换离子回旋共振质谱(Fourier transform ion cyclotron resonance mass spectrometry,FT-ICR MS),从分子水平阐明不同氧化还原条件下土壤剖面中DOC转化的内在规律。研究发现:深层土壤的DOC来源以上层淋溶为主。土壤DOC的平均m/z、芳香指数(Aromatic index,AI)、O/C和双键当量(Double bond equivalent,DBE)随土壤深度的增加而减小。随着土壤深度的增加,反应过程中被降解的DOC分子DBE范围明显缩小(从0~18缩减至0~9),说明土壤对DOC的降解能力随着深度的增加有明显的下降。有氧培养后的DOC分子比无氧培养后的DOC分子具有更高的分子量、芳香性和不饱和度,且脂质的相对丰度比无氧组更低而木质素的相对丰度比无氧组更高,说明有氧条件可同步促进DOC分子的降解和生成。展开更多
A data processing combination of manual and automatic steps for mass peaks identification of a coking gas oil was illustrated.Some representative compounds were identified by manual process.A program was performed to ...A data processing combination of manual and automatic steps for mass peaks identification of a coking gas oil was illustrated.Some representative compounds were identified by manual process.A program was performed to search the various types with the same hetero-atoms(familes-class,NnSsOo)but different rings plus double bonds(R+DB)value(Z in CcH2c+ZNnOoSs),then,alkylation series of each types were revealed by multiplying each mass by 14.00000 in Kendrick mass scale.Finally,isotope groups of each identified peaks were picked up respectively.The method is appropriate to the data analysis of FT-ICR MS spectra with a poor mass accuracy.展开更多
文摘Biological mass spectrometry has received a great progress in recent years.The osteopontin(OPN) isolated and purified from the human milk was studied by HPLC using SCX and C4 columns.After hydrolyzing the purified OPN sample by trypsin,the correlative polypeptide fragments GDSVVYGLR and QNLLAPQTLPSK were obtained by FT-ICR-MS.It showed that the method of nano-spray HPLC combined with FT-ICR-MS and Mascot search was very efficient for the analysis of the purified OPN and its polypeptide fragments.Further study provides more academic theories of their different modifications and the relative bioactivities.
文摘FT-ICR-MS technology has significant sensitivity and dynamic range,enabling the detection of different fragmentations of peptides and proteins at lower and lower levels.In the bottom-up approach,by far the most frequently used proteomics approach,a single LC-MS run can reveal tens and even hundreds of useful information.For each peptide selected for MS/MS,two data-files were generated,one for ECD and another one for CAD.They were merged as described and submitted to the Mascot search engine using the protein database.These thresholds ensure almost 100% statistical confident in the peptide identification.
文摘The phosphorothioate oligonucleotides are used more and more for cancer treatment.Fast analysis of phosphorothioate oligonucleotide is important for quality control of this drug.In this paper,FT-ICR-MS was used to analyze a phosphorothioate oligonucleotide with 6 321 u.Experimental results showed that accurate relative molecular mass of phosphorothioate oligonucleotide determined by FT-ICR-MS can be used for confirmation of its composition.
基金Supported by the Project from Scientific Bureau of Jilin Province, China(No.200705391)
文摘Milk as a key element for infant nutrition represents the only source of feeding for newborns and infants, breast-feeding milk normally contains several bioactive proteins or peptides useful for the development of the immune system that protects infants from diseases. Osteopontin（OPN） plays a distinct role during the processes of lactation, Some studies on OPN isolated and purified from the human milk via HPLC on SCX and Ca columns adopted biological mass spectrometry. After digesting the purified OPN sample with trypsin, the typical correlative polypeptide fragments GDSVVYGLR and QNLLAPQTLPSK are identified by FT-ICR-MS. The rapid identification of OPN is assumed to be reasonably well behaving in a standard bottom-up experiment. It shows that nano-spray HPLC combined with FT-ICR-MS and Mascot search can be used as a high efficient method for the identification of purified OPN and its polypeptide fragments. Further study will provide more academic theories of their different modifications and the bioactivity as well.
基金supported by the National Natural Science Foundation of China (20035010 and 20175033) and Instrumental Innovation Project of Chinese Academy of Sciences.
文摘The coupling of capillary electrophoresis to electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) was presented for the on-line separation and detection of mixture of peptides. With the ultra-high resolution and unmatchable mass measurement accuracy FT-ICR-MS provides, the separation and identification of angiotensin III, octreotide and elastin chemotactic were successfully achieved using this fabricated device, which showed its great application potential in detection and structural identification for multicomponent sample.
文摘为了认识稠油开发过程中低温氧化与高温氧化阶段原油变化规律,利用静态氧化釜开展稠油的高低温氧化实验,借助傅里叶变换离子回旋共振质谱分析技术对高低温氧化前后的原油分子量及O、N、S杂原子化合物特征开展研究,结果表明:原油低温氧化阶段分子量分布特征与原样相似,相对分子量分布范围在200~750,整体呈平缓状单峰型分布,高温氧化阶段分子量分布范围前移,呈明显的前峰单峰型分布;杂原子化合物中的O元素在低温氧化阶段主要以无环的饱和二元酸形式存在,在高温氧化阶段受环化、芳构化及脱甲基作用的影响,伴随着侧链烷基及杂原子基团的断裂和芳构化过程,造成原油中杂原子化合物向着碳数更小、双键当量(double bond equivalents,DBE)值更低的方向演化。该研究探索了温度与原油结构及化学组成之间的关系,对于指导稠油开发现场具有重要意义。
文摘溶解性有机碳(Dissolved organic carbon,DOC)是农田土壤碳库中最重要的活性碳组分。DOC可为土壤微生物提供必需的营养元素,也会诱导复杂的环境效应。本研究以中国青岛市大沽河农业区为研究对象,利用室内培养实验,并结合傅里叶变换离子回旋共振质谱(Fourier transform ion cyclotron resonance mass spectrometry,FT-ICR MS),从分子水平阐明不同氧化还原条件下土壤剖面中DOC转化的内在规律。研究发现:深层土壤的DOC来源以上层淋溶为主。土壤DOC的平均m/z、芳香指数(Aromatic index,AI)、O/C和双键当量(Double bond equivalent,DBE)随土壤深度的增加而减小。随着土壤深度的增加,反应过程中被降解的DOC分子DBE范围明显缩小(从0~18缩减至0~9),说明土壤对DOC的降解能力随着深度的增加有明显的下降。有氧培养后的DOC分子比无氧培养后的DOC分子具有更高的分子量、芳香性和不饱和度,且脂质的相对丰度比无氧组更低而木质素的相对丰度比无氧组更高,说明有氧条件可同步促进DOC分子的降解和生成。
文摘A data processing combination of manual and automatic steps for mass peaks identification of a coking gas oil was illustrated.Some representative compounds were identified by manual process.A program was performed to search the various types with the same hetero-atoms(familes-class,NnSsOo)but different rings plus double bonds(R+DB)value(Z in CcH2c+ZNnOoSs),then,alkylation series of each types were revealed by multiplying each mass by 14.00000 in Kendrick mass scale.Finally,isotope groups of each identified peaks were picked up respectively.The method is appropriate to the data analysis of FT-ICR MS spectra with a poor mass accuracy.
