建立了全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)分析卷烟主流烟气中中性化学成分的方法。以较长的弱极性柱HP-5MS(50 m×0.2 mm i.d.×0.33μm)作为第一维柱,较短的薄液膜中等极性柱DB-17MS(1.7 m×0.1 mm i.d....建立了全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)分析卷烟主流烟气中中性化学成分的方法。以较长的弱极性柱HP-5MS(50 m×0.2 mm i.d.×0.33μm)作为第一维柱,较短的薄液膜中等极性柱DB-17MS(1.7 m×0.1 mm i.d.×0.1μm)作为第二维柱,对优质烟叶单料卷烟烟气的中性成分进行定性分析,经过人工纠错等分析初步鉴定出匹配度大于700的1 464种成分,重点讨论了中性香味羰基化合物全二维点阵的谱图特征,为烟气和复杂体系的深入研究提供了方法学基础。展开更多
基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量...基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。展开更多
保健酒是以白酒或其他酒类为基酒,佐以中药材,对人体具有保健功效的酒饮料。中国劲酒是保健酒的代表产品之一,通常以清香型小曲酒为基酒,加入淮山药、仙茅、当归、肉苁蓉、枸杞子、黄芪、淫羊藿等药材经过现代提取与分离技术调配制成。...保健酒是以白酒或其他酒类为基酒,佐以中药材,对人体具有保健功效的酒饮料。中国劲酒是保健酒的代表产品之一,通常以清香型小曲酒为基酒,加入淮山药、仙茅、当归、肉苁蓉、枸杞子、黄芪、淫羊藿等药材经过现代提取与分离技术调配制成。采用液-液萃取结合全二维气相色谱-飞行时间质谱联用仪(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOF MS)对2种中国劲酒基酒的挥发性成分进行分析,测定其化合物的种类和含量。结果表明:2种中国劲酒基酒中初步定性出挥发性化合物175种,标准品定性化合物40种,其中醇类化合物41种、酯类化合物53种、醛酮类化合物24种、缩醛类化合物2种、酸类化合物24种、呋喃类化合物8种、酚类化合物3种、内酯类化合物8种、含氮化合物8种、含硫化合物1种和酸酐类化合物2种;含氮和含硫化合物在中国劲酒中为首次发现。液-液萃取结合GC×GC-TOF MS技术的分析方法可快速、准确分析鉴定出中国劲酒基酒中挥发性成分,结果旨在为中国劲酒的重要风味物质研究提供参考。展开更多
High resolution mass spectrometry in combination with distillation and SARA fractionation provides us an opportunity for in-depth understanding about the hydrotreating process at the molecular level. In this study, th...High resolution mass spectrometry in combination with distillation and SARA fractionation provides us an opportunity for in-depth understanding about the hydrotreating process at the molecular level. In this study, the atmospheric residue derived from Arabian heavy crude and its hydrotreated products were initially subjected to distillation and SARA fractionation. The saturates were characterized by GC FI/FD TOF MS. The aromatics and resins were characterized by APPI FT-ICR MS. Compositional changes of different compounds (paraffins, naphthenes, aromatic hydrocarbons, and heteroatomic compounds) contained in different distillates (vacuum gas oil, vacuum residue) were obtained. More detailed knowledge about the hydrotreating process was achieved.展开更多
文摘建立了全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)分析卷烟主流烟气中中性化学成分的方法。以较长的弱极性柱HP-5MS(50 m×0.2 mm i.d.×0.33μm)作为第一维柱,较短的薄液膜中等极性柱DB-17MS(1.7 m×0.1 mm i.d.×0.1μm)作为第二维柱,对优质烟叶单料卷烟烟气的中性成分进行定性分析,经过人工纠错等分析初步鉴定出匹配度大于700的1 464种成分,重点讨论了中性香味羰基化合物全二维点阵的谱图特征,为烟气和复杂体系的深入研究提供了方法学基础。
文摘基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。
文摘保健酒是以白酒或其他酒类为基酒,佐以中药材,对人体具有保健功效的酒饮料。中国劲酒是保健酒的代表产品之一,通常以清香型小曲酒为基酒,加入淮山药、仙茅、当归、肉苁蓉、枸杞子、黄芪、淫羊藿等药材经过现代提取与分离技术调配制成。采用液-液萃取结合全二维气相色谱-飞行时间质谱联用仪(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOF MS)对2种中国劲酒基酒的挥发性成分进行分析,测定其化合物的种类和含量。结果表明:2种中国劲酒基酒中初步定性出挥发性化合物175种,标准品定性化合物40种,其中醇类化合物41种、酯类化合物53种、醛酮类化合物24种、缩醛类化合物2种、酸类化合物24种、呋喃类化合物8种、酚类化合物3种、内酯类化合物8种、含氮化合物8种、含硫化合物1种和酸酐类化合物2种;含氮和含硫化合物在中国劲酒中为首次发现。液-液萃取结合GC×GC-TOF MS技术的分析方法可快速、准确分析鉴定出中国劲酒基酒中挥发性成分,结果旨在为中国劲酒的重要风味物质研究提供参考。
基金supported by the National Basic Research Program of China (2010CB226901)
文摘High resolution mass spectrometry in combination with distillation and SARA fractionation provides us an opportunity for in-depth understanding about the hydrotreating process at the molecular level. In this study, the atmospheric residue derived from Arabian heavy crude and its hydrotreated products were initially subjected to distillation and SARA fractionation. The saturates were characterized by GC FI/FD TOF MS. The aromatics and resins were characterized by APPI FT-ICR MS. Compositional changes of different compounds (paraffins, naphthenes, aromatic hydrocarbons, and heteroatomic compounds) contained in different distillates (vacuum gas oil, vacuum residue) were obtained. More detailed knowledge about the hydrotreating process was achieved.
