可食用香料产品质量一致性评价能够保证食品风味一致性。本文基于傅里叶变换离子回旋共振质谱(Fourier Transform Ion Cyclotron Resonance Mass Spectrometry,FT-ICR-MS)结合不添加内标物的手动进样策略建立了一种快速分析香料质量的方...可食用香料产品质量一致性评价能够保证食品风味一致性。本文基于傅里叶变换离子回旋共振质谱(Fourier Transform Ion Cyclotron Resonance Mass Spectrometry,FT-ICR-MS)结合不添加内标物的手动进样策略建立了一种快速分析香料质量的方法,采用降噪、插值与归一化预处理质谱数据,相关系数法筛选样品重复测试中的异常值,主成分分析法评价插值后数据的质量,以验证压缩数据是否具有可行性。结果表明,正离子模式下香料A和香料B的未稀释样品分别被划分到甲醇体积分数0%~2%与0%~3%范围内,实际生产中可将此范围内的样品认定为质量合格。负离子模式样品响应低,优先考虑正离子模式评价可食用香料。展开更多
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
文摘可食用香料产品质量一致性评价能够保证食品风味一致性。本文基于傅里叶变换离子回旋共振质谱(Fourier Transform Ion Cyclotron Resonance Mass Spectrometry,FT-ICR-MS)结合不添加内标物的手动进样策略建立了一种快速分析香料质量的方法,采用降噪、插值与归一化预处理质谱数据,相关系数法筛选样品重复测试中的异常值,主成分分析法评价插值后数据的质量,以验证压缩数据是否具有可行性。结果表明,正离子模式下香料A和香料B的未稀释样品分别被划分到甲醇体积分数0%~2%与0%~3%范围内,实际生产中可将此范围内的样品认定为质量合格。负离子模式样品响应低,优先考虑正离子模式评价可食用香料。
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.
