An excellent analytical tool for the separation and analysis of TCM(Traditional Chinese Medicine) by using HR ESI TOF MS(High Resolution Electrospray Ionization Time of flight Mass Spectrometry) was developed. A home ...An excellent analytical tool for the separation and analysis of TCM(Traditional Chinese Medicine) by using HR ESI TOF MS(High Resolution Electrospray Ionization Time of flight Mass Spectrometry) was developed. A home built HR ESI TOF MS was applied to detect fat soluble components in Danshen( Salvia miltiorrhiza Bage ) directly. Compared with the method of HPLC ESI MS(High Performance Liquid Chromatograph Electrospray ionization Mass Spectrometry) method, HR ESI TOF MS method is more accurate, quick, simple and reliable, so the method can become an effective tool for the quality control of TCM.展开更多
运用反相高效液相色谱(RP-HPLC)对酶解螺蛳腹足肌得到的血管紧张素转换酶(ACE)抑制肽进行两步分离提纯,第一步主要得到8个组分;选取其中活性最高的组分进一步分离,得到2个组分,其中活性较高组分的ACE半抑制浓度为43.5μm o l/L,基本为...运用反相高效液相色谱(RP-HPLC)对酶解螺蛳腹足肌得到的血管紧张素转换酶(ACE)抑制肽进行两步分离提纯,第一步主要得到8个组分;选取其中活性最高的组分进一步分离,得到2个组分,其中活性较高组分的ACE半抑制浓度为43.5μm o l/L,基本为单一肽组分。对提纯的组分分别使用高效液相色谱/电喷雾离子质谱法(HPLC/E S I-M S)和基质辅助激光解吸电离飞行时间质谱法(MALD I-TO F M S)进行分析,同时结合氨基酸组成分析结果,最终得到的肽链一级结构为Lys-G lu-Ile-Trp(KE IW),符合已知的高活性ACE抑制肽的结构规律。经过对两种方法分析过程的比较,认为E S I-M S可以得到多方面的信息,但无法确定肽的序列;MALD I-TO F M S可以得到精确的二级质谱图(m/z精确至0.000 1),从而可以得到确定的肽的序列。展开更多
建立了超高效液相色谱-四极杆飞行时间质谱非靶向快速筛查西红柿中三唑类杀菌剂的方法。样品用乙腈提取、QuEChERS净化、BEH C 18(100 mm×2.1 mm,1.7μm)色谱柱分离,以乙腈和水(均含0.1%(v/v)甲酸)为流动相进行梯度洗脱,采用四极...建立了超高效液相色谱-四极杆飞行时间质谱非靶向快速筛查西红柿中三唑类杀菌剂的方法。样品用乙腈提取、QuEChERS净化、BEH C 18(100 mm×2.1 mm,1.7μm)色谱柱分离,以乙腈和水(均含0.1%(v/v)甲酸)为流动相进行梯度洗脱,采用四极杆飞行时间质谱仪进行检测。质谱离子源为电喷雾电离源,采集方式为正离子数据非依赖分析MS E扫描模式。将19种三唑类杀菌剂按化学结构的不同分为8类。首先通过对8类典型三唑类杀菌剂中代表性的8种标准品的二级质谱图进行分析,总结出三唑类杀菌剂经碰撞诱导解离后产生的特征碎片离子和特征中性碎片丢失的质谱裂解规律,然后再利用另外11种三唑类杀菌剂标准品进行验证,并用于16份北京市售西红柿的非靶向筛查,在1份样品中筛查出烯唑醇。该方法快速、简便、准确率高,可为食品中三唑类杀菌剂残留的筛查提供参考。展开更多
Owing to having very strong bioactivity, oligo-peptides can be used as the medication or the pre-medication and become the studying focus now. Existing methods for synthesizing oligo-peptides included liquid phase pep...Owing to having very strong bioactivity, oligo-peptides can be used as the medication or the pre-medication and become the studying focus now. Existing methods for synthesizing oligo-peptides included liquid phase peptide synthesis, solid phase peptide synthesis and enzymatic peptide synthesis. In this paper, a new method for synthesizing oligo-peptides by phosphorus oxychloride activation was reported. With the assistance of phosphorus oxychloride, the phosphorylation of L-valine could take place and then was assembled into oligo-peptides, which were analyzed by electrospray ionization mass spectrometry(ESI-MS). On quenching with methanol, the reaction mixtures, which were produced under different reaction conditions, yielded the corresponding peptide methyl esters. Moreover, we found that, as the reaction conditions such as reaction time, solvent and temperature were changed, the length of peptides changed. And the length of peptides could be controlled by changing the reaction conditions.展开更多
文摘An excellent analytical tool for the separation and analysis of TCM(Traditional Chinese Medicine) by using HR ESI TOF MS(High Resolution Electrospray Ionization Time of flight Mass Spectrometry) was developed. A home built HR ESI TOF MS was applied to detect fat soluble components in Danshen( Salvia miltiorrhiza Bage ) directly. Compared with the method of HPLC ESI MS(High Performance Liquid Chromatograph Electrospray ionization Mass Spectrometry) method, HR ESI TOF MS method is more accurate, quick, simple and reliable, so the method can become an effective tool for the quality control of TCM.
文摘运用反相高效液相色谱(RP-HPLC)对酶解螺蛳腹足肌得到的血管紧张素转换酶(ACE)抑制肽进行两步分离提纯,第一步主要得到8个组分;选取其中活性最高的组分进一步分离,得到2个组分,其中活性较高组分的ACE半抑制浓度为43.5μm o l/L,基本为单一肽组分。对提纯的组分分别使用高效液相色谱/电喷雾离子质谱法(HPLC/E S I-M S)和基质辅助激光解吸电离飞行时间质谱法(MALD I-TO F M S)进行分析,同时结合氨基酸组成分析结果,最终得到的肽链一级结构为Lys-G lu-Ile-Trp(KE IW),符合已知的高活性ACE抑制肽的结构规律。经过对两种方法分析过程的比较,认为E S I-M S可以得到多方面的信息,但无法确定肽的序列;MALD I-TO F M S可以得到精确的二级质谱图(m/z精确至0.000 1),从而可以得到确定的肽的序列。
文摘Owing to having very strong bioactivity, oligo-peptides can be used as the medication or the pre-medication and become the studying focus now. Existing methods for synthesizing oligo-peptides included liquid phase peptide synthesis, solid phase peptide synthesis and enzymatic peptide synthesis. In this paper, a new method for synthesizing oligo-peptides by phosphorus oxychloride activation was reported. With the assistance of phosphorus oxychloride, the phosphorylation of L-valine could take place and then was assembled into oligo-peptides, which were analyzed by electrospray ionization mass spectrometry(ESI-MS). On quenching with methanol, the reaction mixtures, which were produced under different reaction conditions, yielded the corresponding peptide methyl esters. Moreover, we found that, as the reaction conditions such as reaction time, solvent and temperature were changed, the length of peptides changed. And the length of peptides could be controlled by changing the reaction conditions.
