CZE ESI MS is one of the most sensitive detection method and one of the potential method for protomics analysis. In this work, peptide mixture was separated and detected by using CZE ESI MS, and the influence of pH va...CZE ESI MS is one of the most sensitive detection method and one of the potential method for protomics analysis. In this work, peptide mixture was separated and detected by using CZE ESI MS, and the influence of pH value of buffer and composition of sheath liquid on CE separation and MS detection was investigated. The method allows the detection limits up to 4 2—33 pg. The result of this method is better than that of CE UV for the peptide analysis.展开更多
A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （urid...A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.展开更多
针对现有污水样本快速检测技术存在的不足,以及传统实验室质谱技术无法应用于现场快速检测、检测耗时较长等问题,本文提出了一种基于脉冲直流电喷雾电离质谱(pulsed-DC-ESI-MS)测定生活污水中11种常见毒品(吗啡、甲基苯丙胺、去甲氯胺...针对现有污水样本快速检测技术存在的不足,以及传统实验室质谱技术无法应用于现场快速检测、检测耗时较长等问题,本文提出了一种基于脉冲直流电喷雾电离质谱(pulsed-DC-ESI-MS)测定生活污水中11种常见毒品(吗啡、甲基苯丙胺、去甲氯胺酮、苯丙胺、3,4-亚甲基双氧甲基苯丙胺、可卡因、6-单乙酰吗啡、3,4-亚甲基双氧苯丙胺、苯甲酰爱康宁、氯胺酮、可待因)的快速检测方法。污水样品经浓盐酸调节pH至2,用Oasis PRiME MCX固相萃取柱进行萃取,萃取液经氮吹至近干后用200μL甲醇复溶,涡旋0.5 min;复溶后的样品溶液经0.22μm有机相滤膜过滤后采用pulsed-DC-ESI-MS进行分析。方法学验证结果表明,11种毒品在各自的线性范围内具有良好的线性关系,相关系数(r2)均≥0.9986,检出限(LOD)为0.01~0.5μg/L,定量限(LOQ)为0.05~5μg/L。在低、中、高3个加标水平下,11种毒品的回收率为88.0%~107.6%,日内和日间精密度均≤8.5%。该方法检测速度快,大大提高了检测效率,适用于生活污水中常见毒品的快速检测分析。展开更多
利用DNA重组技术在柞蚕蛹中表达重组人促红细胞生成素(Recombinant human erythropoietin,rhEPO),经过亲和层析纯化后,用SDS-PAGE分离纯化各组分,并通过电喷雾电离串联质谱技术(ESI-MS/MS)检测其糖基化修饰.结果显示,在柞蚕蛹中表达的rh...利用DNA重组技术在柞蚕蛹中表达重组人促红细胞生成素(Recombinant human erythropoietin,rhEPO),经过亲和层析纯化后,用SDS-PAGE分离纯化各组分,并通过电喷雾电离串联质谱技术(ESI-MS/MS)检测其糖基化修饰.结果显示,在柞蚕蛹中表达的rhEPO比活性约为1190 U/μg,其糖基化修饰位点与人体表达的EPO一致,有3个N-糖基化位点和1个O-糖基化位点.凝集素杂交实验结合质谱结果表明,柞蚕蛹表达的rhEPO的糖链中缺乏唾液酸修饰,而缺少唾液酸修饰的EPO通过鼻腔给药后在多种神经系统疾病的治疗中发挥着重要的作用.所得结果为进一步研究外源蛋白在柞蚕蛹-柞蚕核型多角体病毒(Anthraea pernyi nucleopolyhedrorirus,ApNPV)宿主载体表达系统表达后的糖基化与生物活性提供了依据.展开更多
文摘CZE ESI MS is one of the most sensitive detection method and one of the potential method for protomics analysis. In this work, peptide mixture was separated and detected by using CZE ESI MS, and the influence of pH value of buffer and composition of sheath liquid on CE separation and MS detection was investigated. The method allows the detection limits up to 4 2—33 pg. The result of this method is better than that of CE UV for the peptide analysis.
文摘A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.
文摘针对现有污水样本快速检测技术存在的不足,以及传统实验室质谱技术无法应用于现场快速检测、检测耗时较长等问题,本文提出了一种基于脉冲直流电喷雾电离质谱(pulsed-DC-ESI-MS)测定生活污水中11种常见毒品(吗啡、甲基苯丙胺、去甲氯胺酮、苯丙胺、3,4-亚甲基双氧甲基苯丙胺、可卡因、6-单乙酰吗啡、3,4-亚甲基双氧苯丙胺、苯甲酰爱康宁、氯胺酮、可待因)的快速检测方法。污水样品经浓盐酸调节pH至2,用Oasis PRiME MCX固相萃取柱进行萃取,萃取液经氮吹至近干后用200μL甲醇复溶,涡旋0.5 min;复溶后的样品溶液经0.22μm有机相滤膜过滤后采用pulsed-DC-ESI-MS进行分析。方法学验证结果表明,11种毒品在各自的线性范围内具有良好的线性关系,相关系数(r2)均≥0.9986,检出限(LOD)为0.01~0.5μg/L,定量限(LOQ)为0.05~5μg/L。在低、中、高3个加标水平下,11种毒品的回收率为88.0%~107.6%,日内和日间精密度均≤8.5%。该方法检测速度快,大大提高了检测效率,适用于生活污水中常见毒品的快速检测分析。
