优化流动相提高代谢组学尿液样品中代谢物覆盖率的方法

发布时间：2018-06-09 01:26

本文选题：高效液相色谱串联相飞行时间质谱 + 代谢组学　；参考：《分析试验室》2017年01期

【摘要】：采用高效液相色谱飞行时间质谱(HPLC-QTOF-MS)对尿液进行代谢组学分析,在流动相中分别添加甲酸,甲酸铵,乙酸铵3种流动相改性剂来考察尿液中代谢物的覆盖范围、离子响应强度和分辨率。通过标准品和质控样品评价手段建立了适用于尿液代谢物分析的方法。在该方法基础上,在流动相中分别添加甲酸、甲酸铵、乙酸铵,正负离子模式下尿液中检测到的离子数分别为1452,1197,714和636,593,947。正离子模式下,添加甲酸后的离子质荷比范围最广为m/z 340.0488±125.7661;负离子模式没有明显差别。在正、负离子模式下,在流动相中添加甲酸和乙酸铵,代谢物覆盖率最高,且离子响应强度和分辨率有所提高。方法已应用于复合农药和壬基酚暴露的尿液代谢组学研究以及可能生物标志物的筛选。
[Abstract]:High performance liquid chromatography (HPLC) / time of flight mass spectrometry (HPLC-QTOF-MS) was used to analyze the metabolites of urine. Three kinds of mobile phase modifiers, formic acid, ammonium formate and ammonium acetate, were added to the mobile phase to investigate the coverage of metabolites in urine. Ion response intensity and resolution. A method for the analysis of metabolites in urine was established by means of standard sample and quality control sample evaluation. On the basis of this method, the number of ions detected in urine by adding formic acid, ammonium formate, ammonium acetate and positive and negative ion modes in the mobile phase is 1452 ~ 1197714 and 636593947 respectively. In the positive ion mode, the ion mass charge ratio after formic acid addition is the widest in the range of m / z 340.0488 卤125.7661, but there is no significant difference in the negative ion mode. When formic acid and ammonium acetate were added into the mobile phase, the metabolite coverage was the highest in the positive and negative ion mode, and the ionic response intensity and resolution were improved. The method has been applied to the study of urinary metabolomics and the screening of possible biomarkers after exposure to compound pesticides and nonylphenol.
【作者单位】：哈尔滨工业大学化工与化学学院;中国农业科学院农业质量标准与检测技术研究所农业部农产品质量安全重点实验室;
【基金】：中国农业科学院科技创新工程“农业化学污染物残留检测及行为研究”创新团队项目中国科技部基础性专项(2013FY110100) 农业公益性行业计划(2012BAK10B05-05)资助
【分类号】：R446.12;O657.63

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