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Identification of Key Odor Compounds from Three Kinds of Wood Species

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Identification of Key Odor Compounds from Three Kinds of Wood Species Qi-Fan Wang, Ya-Li Shao, Tian-Yu Cao and Jun Shen* Identification of Key Odor Compounds from Three Kinds of Wood Species Identification and analysis of key odor compounds from three kinds of wood species by Gas Chromatography-Mass spectroscopy-Olfactometry Abstract: In order to solve the problem of indoor odor and better understand the chemical composition and sources of odor from solid wood, we collected the volatile substances from Populus ussuriensis Kom, Pinus sylvestris var, mongolica Litv, and Tilia amurensis Rupr, using the Micro-Chamber/Thermal Extractor and Gas Chroma- tography-Mass spectroscopy-Olfactometry. Results showed that: The main odor compounds of Populus ussuriensis Kom were aromatics (1 kind), aldehydes (1 kind), the main odor compounds of Pinus sylvestris var, mongolica Litv, were aromatic (2 kinds), alkenes (8 kinds), alcohols (4 kinds) and aldehydes (1 kind). The main odor compounds of Tilia amurensis Rupr, were alkenes (2 kinds), alcohols (1 kind), alde- hydes (1 kind). At the same time, 7 kinds unknown compounds were detected from Populus ussuriensis Kom., which appeared at 9.02, 9.7, 20.6, 25.03, 28.82, 32.88, and 34.58 minutes, with the odor of sweet, plastic&spicy, special, stimulat- ing&burning&plastic&spicy, stinky, plastic&spicy and plastic, respectively. 6 kinds unknown compounds were detected from and Tilia amurensis Rupr., which ap- peared at 5.70, 9.73, 9.92, 30.27, 30.9, and 32.38 minutes and presented as stinky, plastic&stinky, earthy, stinky, delightful, and aromatic. The emergence times of odor compounds focused around 5 to 12 minutes and 18 to 36 minutes. The volatile substances of Populus ussuriensis Kom, Pinus sylvestris var, mongolica Litv, and Tilia amurensis Rupr, were 25, 27 and 40 kinds corresponding, with the key odor com- pounds of alkenes, aldehydes, and alcohols. The odor intensity of VOCs from the three wood species did not show a positive correlation with the concentrations. The aroma of three kinds of wood species are composed of several aroma-active volatile || Qi-Fan Wang, Northeast Forestry University, 26 Hexing Road, Harbin 150040, China. Email: [email protected] Ya-Li Shao, Northeast Forestry University, 26 Hexing Road, Harbin 150040, China. Email: [email protected] Tian-Yu Cao, Northeast Forestry University, 26 Hexing Road, Harbin 150040, China. Email: [email protected] Jun Shen, Northeast Forestry University, 26 Hexing Road, Harbin 150040, China. Email: [email protected] DOI 10.1515/9783110540048-011, © 2017 Jun Shen et al, published by De Gruyter. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivs 3.0 License. 102 | Wang, Shao, Cao, Shen components which can affect the overall flavor for their low threshold. Keywords: Chromatography-Mass spectroscopy-Olfactometry; Populus ussuriensis Kom; Pinus sylvestris var, mongolica Litv; Tilia amurensis Rupr; Key odor compounds 1 Introduction In recent years, people are increasingly using wood materials in their interior deco- rating because of its natural affinity and visual sense of harmony. The release of volatile organic compounds (VOCs) in indoor air is therefore increasing. Organic compounds can release either pleasant or irritating odors into the surrounding envi- ronments. These odors are composed of a variety of single compounds, and some of those compounds may be harmful to human’s health. Gas chromatography–mass spectroscopy olfactometry (GC-MS-O) is improved from the GC-MS by detecting VOCs emissions from wood and combining the separation ability of GC-MS with the sensitive olfactory ability of humans. GC-MS-O separates the various VOCs compo- nents and uses our noses as detectors [1] to evaluate each compound, separately. Based on the sensitivity of the human sense of smell, which can exceed that of other chemical detectors, GC-MS-O was used to select and evaluate active odor substances from complex mixtures of VOCs [2]. This method is helpful in identifying key odor compounds and determining the intensity of those compounds. GC-MS-O was first proposed in 1964 [3, 4]. It was performed by smelling the out- flow components of GC-MS directly. This method combined not only the GC-MS advantages of high separation efficiency, strong qualitative ability, high sensitivity, and quantitative accuracy but also the sensory evaluation of humans. In 1976, Acree et al. improved the original GC-MS-O technology by adding humid air and by smell- ing the GC outflow after film chromatography processing. In the mid-1980s, Acree and Ullrich [5, 6] used dilution-analysis methods to analyze the intensity of the vari- ous odors at the same time, which made GC-MS-O technology widely applicable in many situations. Currently, there are four major GC-MS-O detection methods [7], the dilution analysis, time–intensity analysis, detection frequency methods, and poste- rior intensity evaluation. With the development of extraction and separation tech- nology, GC-MS-O has been widely used in the research of fruits [8], vegetables [9], dairy products [10], paint [11], gypsum [12], and other fields such as tobaccos, flavor- ing agents and wines. In total, there are many researches on odor emissions, but there is few research- es about the odor emission from wood materials, especially solid woods. The odor problem of interior decoration has impacted people’s life a lot. Usually, we can only smell the overall odor but cannot know the single key odor components that make up the overall odor. This study isolated and indentified the key odor compounds Identification of Key Odor Compounds from Three Kinds | 103 from Populus ussuriensis Kom, Pinus sylvestris var. mongolica Litv. and Tilia amuren- sis Rupr. And at the same time, the characteristics and intensities of the key odor compounds were showed and chemical composition and source of overall odor were found to provide basic data of interior decoration materials. 2 Materials and Methods 2.1 Experimental Materials The essential parameters of the three wood species are presented in Table 1. The samples were cut into round pieces (60 mm diameter) for the microcham- ber/thermal extractor apparatus. The exposed area was 5.65 × 10−3 m2. After the edg- es of specimen were sealed with aluminum foil to prevent the release of compounds. The samples were stored in Teflon bags and placed in a refrigerator until needed. 2.2 Experimental Equipments 2.2.1 Sampling Devices Two sampling devices were used. The Micro-Chamber/Thermal Extractor µ-CTE 250 (Markes International Inc., UK) consists of four cylindrical micropools (each with a microcell diameter of 64 mm by a depth of 36 mm). The sampling temperature can be adjusted up to 250 °C. It can test four samples at the same time. The other sam- pling device was a Tenax TA tube (Markes International Inc., UK). In this device, the material of the pipe body is stainless steel, and the sampling tube contains 200 mg of 2, 6-dibenzofurans porous polymer, which can efficiently adsorp or desorp the volatile organic gases. 2.2.2 Detection and Analysis Devices Three detection and analysis devices were used. (i) The Unity thermal analysis desorption unit (Markes International Inc., UK). Nitrogen was used as the carrier gas. The related parameters include: thermal desorption temperature, 280 °C, cold-trap adsorption temperature, −15 °C, and thermal analysis time, 10 minutes; and injection time, 1 minute. (ii) DSQ II series GC-MS (Thermo Scientific, Germany). Chromatography was per- formed with a DB-5 quartz capillary column (3,000 mm by 0.26 mm by 0.25 μm). Helium was used as the carrier gas with a constant velocity of 1.0 mL/min by splitless injection. The chromatographic column was initially kept at 40 °C for 2 104 | Wang, Shao, Cao, Shen minutes; then, the temperature was increased to 50°C (in 2 °C/min increments) and was held for 4 minutes. Finally, the temperature was elevated to 250 °C (in 10 °C/min increments) and held for 8 minutes. The injection port temperature was 250 °C. The following GC-MS conditions were applied: ionization mode, electron ionization (EI); ion energy, 70 eV; transmission line temperature, 270 °C; ion source temperature, 230 °C; and mass scan range, 50 to 650 atomic mass units. (iii) Sniffer 9000 Olfactory Detector (Brechbühler, Switzerland). Combined with GC or GC-MS, the quantitative and qualitative analyses can be made, and the com- pound’s odor intensity can be reflected directly and recorded. The effluent of the GC capillary is divided into two parts, one part enters the mass spectrometer, and the other part is used for sensory evaluation (ratio 1:1). The transmission line temperature was 150 °C, and nitrogen was used as the carrier gas through a purge valve. Humid air was added to prevent dehydration of the nasal mucosa. 2.3 Experimental Method 2.3.1 Sampling Method The experiment used the Tenax TA sampling tubes tubes to adsorb VOCs from dif- ferent wood species under constant experimental conditions (sampling temperature, 40 °C; ratio of air exchange rate to loading factor, 0.5; air flow rates, 47 mL/min). Four samples were collected under these conditions, with a sampling cycle of 8 hours. Each sample’s contents were 3 liters. After sampling, the Tenax TA sampling tubes were wrapped in teflon plastic bags until needed. 2.3.2 Analytical Method Two analytical methods were used. GC-MS and its built-in software were used to analyze the VOCs. The MS detection peak used the 2008 spectral library of the Na- tional Institute of Standards and Technology (NIST) (matching degrees up to 800 °C or above). An internal-standard method was used in this experiment, with deuteri- um substituted for toluene at a concentration of 200 ng/μL, which added 2 μL.
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