Determination of Formaldehyde in Urine by Headspace Gas Chromatography

Abstract

Formaldehyde is a carcinogen to which humans are exposed daily, but few methods are available to quantify formaldehyde in biological samples. We developed a simple, sensitive and rapid technique for the quantification of formaldehyde in urine by derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine, using a headspace sampler coupled to a gas chromatograph equipped with an electron capture detector. The detection limit was 1.08 microg/L. The overall recovery of formaldehyde spiked in urine was 99%. The concentration of formaldehyde in urine obtained from healthy volunteers ranged from 56.85 to 144.57 microg/L. This method can be used successfully to measure formaldehyde in urine.

A Fluorogenic Probe for Ultrafast and Reversible Detection of Formaldehyde in Neurovascular Tissues

“…To better understand the Janus biological properties of FA, it is essential to have practical methods and tools to detect dynamic changes of FA in vivo . Traditional methods for FA analysis have relied on in vitro techniques, including gas chromatography 15, 16, high-performance liquid chromatography 17, 18, selected ion flow tube mass spectrometry 19, 20, and radiometry 21. Although these methods have facilitated FA biology study to some extent, they nevertheless suffer from tedious biological sample preparation procedures and the intrinsic inability to detect FA in complex live biological systems.…”

Liquid chromatography–tandem mass spectrometry for the determination of low-molecular mass aldehydes in human urine

“…The results obtained by the proposed method warrant the following comments: (i) the method extends the scope of MS/MS detection in the determination of LMMAs in urine samples by LC after their DNPH derivatization: to our knowledge, the small number of published papers on this topic has been focused on the determination of one/few aldehydes in other biological matrices [19,20] with only one in urine samples [21]; in any case a systematic quantitative analysis including recovery studies has been not carried out; (ii) the continuous SPE system proposed overcomes the main shortcomings associated with the use of DNPH [22] as derivatizing agent for the determination of aldehydes: high temperatures and in acidic medium, high reaction times, and the use of an additional LLE or SPE step required prior to LC separation. As a result, the whole analytical process is simple and subsequently the analysis time is shortened for the DNPH-LC-ESI-MS/MS method proposed; (iii) the LODs and LOQs afforded by combining the SPE step and MS/MS detection (15-65 ng/l and 50-200 ng/l) are lower than those provided by recent GC alternatives with MS [3,13,14] or electron capture [8] detection for the analysis of these carbonyl compounds in urine samples. In summary, the method is a powerful and robust alternative for quantification of LMMAs with an excellent LOD, accuracy and precision and is capable of detecting these aldehydes in human urine samples at levels as low as nanogram-per-litre.…”

“…Owing to their volatility and activity, derivatization is often required although direct analysis has also been used, as in the monitoring of urinary acrolein concentration by headspace (HS) [5] or by HS/solid-phase microextraction (SPME) [6,7] coupled to GC with mass spectrometric (MS) detection. Via derivatization, hydrazine reagents such as pentafluoro- [12] and 2,4,6-trichlorophenylhydrazine [3,13] or O-(2,3,4,5,6-pentafluobenzyl) hydroxylamine [8,14] have been used as labels for the determination of the aldehydes in urine as biomarkers of LPO in polyunsaturated lipids [3,[12][13][14] or as indicators of exposure to these chemicals [8]. An additional liquid-liquid extraction (LLE) step with n-hexane is usually required for the cleanup and preconcentration of derivatization products prior to their separation by GC [3,12,14].…”

“…Thus, urinary aldehydes have mainly been used to study lipid peroxidation (LPO)-induced DNA damage in cancer diseases [2][3][4] and for the determination of acrolein, the metabolite of the anticancer drugs cyclophosphamide and ifosfamide, which causes hemorrhagic cystitis [5][6][7]. Additionally, these aldehydes have also been detected in urine as indicators of their presence [8], as biomarkers in bladder and prostate cancer [9,10] and as metabolites formed in semicarbazide-sensitive amine-mediated deamination in diabetic complications [11].…”

Formation of the diuretic chlorazanil from the antimalarial drug proguanil—Implications for sports drug testing

“…[10], some of which have been described as compounds regularly eliminated into human urine under specific dietary, environmental/occupational, and/or health conditions [19][20][21][22][23][24]. In order to test the hypothesis, the reactivity of N-(4-chlorophenyl)-biguanide with different chemicals was assessed in methanol in accordance to literature protocols [10] Figure 2.…”