通过纤维上衍生化、固相微萃取和气相色谱-质谱联用技术测定人体呼出气体中的醛类物质。
Determination of aldehydes in human breath by on-fibre derivatization, solid-phase microextraction and GC-MS.
作者信息
Svensson Sophie, Lärstad Mona, Broo Klas, Olin Anna-Carin
机构信息
Occupational and Environmental Medicine, Sahlgrenska University Hospital and Academy at Göteborg University, Box 414, SE 405 30 Göteborg, Sweden.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Dec 1;860(1):86-91. doi: 10.1016/j.jchromb.2007.10.021. Epub 2007 Oct 22.
A GC-MS method for the simultaneous determination of hexanal, heptanal, octanal, nonanal and decanal in exhaled breath was established and validated. The aldehydes were derivatized on PDMS/DVB fibres using O-2,2,4,5,6-(pentafluorobenzyl) hydroxylamine hydrochloride (PFBHA) as the headspace derivatization reagent. The resultant oximes were quantified by GC-MS in selected ion monitoring (SIM) mode. The method provides detection limits of 0.01-0.03 nM for the aldehydes, with a linear response in the concentration range 0.002-20 nM. Within-day precision values for the five aldehydes at 0.02-0.04 nM and 0.2-0.4 nM were in the ranges: 3-9% and 3-8%, respectively; the corresponding between-day precision values were 11-22% and 10-24%. Exhaled breath samples could be stored at -20 degrees C for 48 h.
建立并验证了一种用于同时测定呼出气中己醛、庚醛、辛醛、壬醛和癸醛的气相色谱 - 质谱联用（GC-MS）方法。使用O-2,2,4,5,6-（五氟苄基）盐酸羟胺（PFBHA）作为顶空衍生试剂，在聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）纤维上对醛类进行衍生化。通过GC-MS在选择离子监测（SIM）模式下对生成的肟进行定量。该方法对醛类的检测限为0.01 - 0.03 nM，在0.002 - 20 nM的浓度范围内具有线性响应。五种醛在0.02 - 0.04 nM和0.2 - 0.4 nM时的日内精密度值分别在3 - 9%和3 - 8%范围内；相应的日间精密度值为11 - 22%和10 - 24%。呼出气样品可在-20℃下储存48小时。
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