Determination of acetone in human breath by gas chromatography-mass spectrometry and solid-phase microextraction with on-fiber derivatization
Determination of acetone in human breath by gas chromatography-mass spectrometry and solid-phase microextraction with on-fiber derivatization
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DOI：
10.1016/j.jchromb.2004.08.013
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发表时间：
2004-10-25
影响因子：
3
通讯作者：
Zhang, XM
中科院分区：
文献类型：
--
作者：
Deng, CH;Zhang, J;Zhang, XM
呼吸丙酮的分析已被用作糖尿病的诊断工具。由于丙酮的挥发性和活性，很难用气相色谱-质谱联用（GC-MS）法准确测定人体呼吸中的丙酮浓度。为了克服这一问题，我们建立了一种新的方法，使用气相色谱-质谱和固相微萃取（SPME）纤维衍生化测定丙酮的人呼吸。将来自对照组和糖尿病患者的呼吸气体收集在3-1 Tedlar袋中。0-2,3,4,5,6-采用65 μ m聚二甲基硅氧烷-二乙烯基苯固相微萃取纤维对盐酸五氟苄基羟胺（PFBHA）溶液进行吸附（PDMS-DVB），然后将纤维在Tedlar袋中在40 ℃下进一步顶空暴露于呼出气体中4 min。最后，将纤维上形成的丙酮肟解吸并通过GC-MS分析。使用外标法，通过测量丙酮肟定量分析人呼吸中的丙酮。该方法对呼吸中丙酮的检出限为0.049ppbv，相对标准偏差（R.S.D.）值为3.4%，准确度极佳。此外，该方法样品制备简单，无需有机溶剂。糖尿病患者呼气中丙酮浓度高于1.71 ppmv，而正常人呼气中丙酮浓度低于0.76 ppmv。结果表明，GC-MS和SPME纤维上衍生法是一种简便、快速、灵敏、无溶剂的测定呼气中低浓度丙酮的方法，呼气中丙酮的分析可作为糖尿病诊断的辅助工具。(C)2004 Elsevier B. V.保留所有权利。
Analysis of breath acetone has been used as a diagnostic tool for diabetes. Due to its nature of volatility and activity, it is very difficult to accurately measure the concentration of acetone in human breath by gas chromatography-mass spectrometry (GC-MS). To overcome this problem, we developed a new method using GC-MS and solid-phase microextraction (SPME) with on-fiber derivatization to determine acetone in human breath. Breath gas from controls and diabetic patients was collected in 3-1 Tedlar bags. 0-2,3,4,5,6-(Pentafluorobenzyl) hydroxylamine hydrochloride (PFBHA) in solution was firstly adsorbed on the SPME fiber of 65 mum polydimethylsiloxane-divinylbenzene (PDMS-DVB), and then the fiber was further headspace exposed in exhaled gas in the Tedlar bag at 40degreesC for 4 min. Finally, the formed acetone oxime on the fiber was desorbed and analyzed by GC-MS. Using external standard method, acetone in the human breath was quantitatively analyzed by measurement of its oxime. The method provided a low detection limit of 0.049 ppbv for acetone in breath, relative standard deviation (R.S.D.) value of 3.4%, excellent accuracy. In addition, the method required simple sample preparation and no organic solvent. Acetone in diabetic breath was found to be higher than 1.71 ppmv, while its concentration in normal breath was lower than 0.76 ppmv. The results show that GC-MS and SPME with on-fiber derivatization is a simple, rapid and sensitive and solvent-free method for determination of low concentration acetone in breath and analysis of breath acetone can be used as supplementary tool for diagnosis of diabetes. (C) 2004 Elsevier B.V. All rights reserved.