过热水蒸气蒸馏−干馏制备杉木烟熏香料及组成分析

doi:10.11707/j.1001-7488.LYKX20250166

Abstract

Abstract:

Objective: In response to the issues of low utilization efficiency of processing residues (such as Chinese fir roots and chips) generated throughout the Chinese fir industrial chain, as well as the challenges of low yield and poor quality of traditional processing techniques for the preparation of smoke flavorings, the integrated technology of superheated steam distillation-cracking process (SSD-CP) was proposed in this study. This study aims to provide innovative solutions for the efficient and high-value utilization of Chinese fir processing residues through directional thermal conversion. Method: In this study, Chinese fir chips were used as the raw material, and experiments were conducted using a self-designed SSD-CP integrated system (including a steam generator, superheating device, cracking unit, and multi-stage condensation system). The distillates at 150–350 ℃ were collected, and the smoke flavoring was obtained by extracting the distillate, dehydrating it, and rotating evaporation to remove the solvent. The chemical composition of the smoke flavorings was analyzed via Gas Chromatography-Mass Spectrometry (GC-MS), and the aroma characteristics were systematically evaluated. Comparative assessments were conducted to assess differences in product yield and quality between steam distillation and dry distillation methods. Result: The smoke flavorings prepared via SSD-CP achieved a yield of 29.45%, which was 39 times higher than that of steam distillation (0.76%) and 4 times higher than that of dry distillation (6.94%), demonstrating a significant enhancement in resource conversion efficiency. The key aroma-contributing components were identified through GC-MS analysis, including α-cedrene, cedrol, 2-methoxy-4-methylphenol, β-cedrene, isoeugenol, guaiacol, α-terpineol, 4-ethyl-2-methoxyphenol, and 5-methyl-2-furaldehyde. In a high-temperature environment, cedrol was able to be converted into alkenes, and cellulose, hemicellulose and lignin generated heterocyclic and phenolic substances through chemical reactions such as pyrolysis and rearrangement, which impart the flavor with strong smoke characteristics. Sensory evaluation revealed that the SSD-CP smoke flavorings presented dominant smoky, caramelized, and woody notes with a subtle cooling sensation, featuring overall transparency and long-lasting. Conclusion: The SSD-CP technology significantly improves the yield of smoke flavorings, and the quality fraction and aroma of its main aroma components are better than those produced by the traditional technology. The technology results in the characteristic aroma of the smoke flavorings with the core of smoky, caramelized, and woody notes. A transformation system of “wood waste to smoke flavorings” has been constructed, and the efficient and high-value utilization of Chinese fir processing residues has been successfully realized.

Key words: Chinese fir chips, smoke flavorings, superheated steam distillation-cracking process integrated technology, composition analysis, comprehensive utilization

CLC Number:

Jiaqi Cai,Xueping Zhang,Ping Mao,Jing Yang,Senwen Yu,Kai Zhu,Kui Zhang,Xu Wang,Haijun Xu. Preparation of Smoke Flavorings of Cunninghamia lanceolata by Superheated Steam Distillation-Cracking and their Composition Analysis[J]. Scientia Silvae Sinicae, 2026, 62(3): 193-200.

Figures/Tables 10

Fig.1

Table 1

Table 2

Table 3

Table 4

Table 5

Chemical composition analysis of flavorings prepared by different methods"

序号 Order number	化合物名称 Chemical name	相对质量分数Relative mass fraction（%）
序号 Order number	化合物名称 Chemical name	水蒸气蒸馏 SD	干馏 CP	过热水蒸气蒸馏? 干馏SSD-CP
1	糠醛Furfural	—	0.37	0.60
2	糠醇Furfuryl alcohol	—	0.11	0.19
3	甲基环戊烯醇酮Methyl cyclopentenolone	—	0.28	0.12
4	5-甲基-2-糠醛5-Methyl-2-furaldehyde	—	0.33	0.50
5	β-蒎烯β-Pinene	—	0.22	—
6	（+）-柠檬烯（+）-Limonene	—	0.54	0.16
7	苯酚Phenol	—	0.47	0.25
8	3-甲基-1，2-环戊二酮3-Methyl-1，2-cyclopentanedione	—	0.91	0.13
9	萜品油烯Terpinolene	—	0.83	—
10	4-异丙烯基甲苯4-Isopropenyltoluene	—	0.81	—
11	邻甲基苯酚o-Cresol	—	0.89	0.41
12	愈创木酚Guaiacol	—	1.18	1.79
13	（$ - $）-樟脑（$ - $）-Camphor	0.33	0.41	—
14	（Z）-水合桧烯（Z）-4-Thujanol	—	0.31	—
15	α-松油醇α-Terpineol	0.78	0.13	0.15
16	2-莰醇2-Camphanol	0.19	0.40	0.19
17	二氢香芹醇Dihydrocarveol	—	0.05	0.11
18	2-甲氧基-4-甲基苯酚2-Methoxy-4-methylphenol	—	8.98	7.69
19	香紫苏醇Sclareol	—	—	0.22
20	人参环氧炔醇Panaxydol	—	0.29	—
21	4-乙基-2-甲氧基苯酚4-Ethyl-2-methoxyphenol	—	0.47	0.87
22	红没药醇α-Bisabolol	—	0.04	0.06
23	异丁香酚Isoeugenol	—	3.20	3.47
24	α-柏木烯α-Cedrene	11.80	34.45	42.30
25	β-柏木烯β-Cedrene	2.58	7.39	7.29
26	α-依兰油烯α-Muurolene	0.31	0.17	1.04
27	γ-古芸烯γ-Gurjunene	—	1.86	2.01
28	α-姜黄烯α-Curcumene	0.15	0.45	0.34
29	α-瑟林烯α-Selinene	0.12	0.54	0.30
30	β-榄香烯β-Elemene	0.86	—	1.04
31	长叶烯Longifolene	0.15	0.26	—
32	罗汉柏烯Thujopsene	—	0.49	0.13
33	β-花柏烯β-Chamigrene	0.11	—	0.06
34	δ-杜松烯δ-Cadinene	0.20	0.07	0.75
35	α-布藜烯α-Bulnesene	—	—	0.12
36	（E）-10-十七烯-8-炔酸甲酯（E）-10-Heptadecen-8-ynoic acid methyl ester	0.27	—	0.05
37	白菖醇Calarene	0.23	0.05	0.02
38	柏木醇Cedrenol	69.31	32.48	24.58
39	γ-桉叶油醇γ-Cineole	0.41	—	0.12
40	T-依兰油醇T-muurolol	0.56	—	0.03
41	α-杜松醇α-Cadinol	1.27	0.02	0.65
42	异瑟模环烯醇Isocembrol	1.06	—	0.19
43	3-乙基-5- （2-乙基丁基） -十八烷3-Ethyl-5-（2-ethylbutyl）octadecane	1.08	—	—
44	角鲨烯Squalene	1.49	—	0.03
45	香叶基香叶醇Geranylgeraniol	2.06	—	0.12
46	1-三十七烷醇1-Heptatriacotanol	1.17	0.02	—
47	枫香脂Ethyl iso-allocholate	3.52	—	—
48	亚油酸Linoleic acid	—	0.08	—
49	顺式-8，11，14-二十碳三烯酸cis-8，11，14-Eicosatrienoic Acid	—	0.04	—
50	香橙烯氧化物 2Aromadendrene oxide 2	—	0.04	0.55
51	莪术烯醇Curcumenol	—	0.04	—
52	5，7-十六碳二炔酸甲酯Methyl 5，7-hexadecadiynoate	—	0.03	0.15
53	西松烯Cembrene	—	0.02	0.27
54	棕榈酸甲酯Methyl palmitate	—	0.03	—
55	（$-$）-扁枝烯（$ - $）-Phyllocladene	—	0.02	0.34
56	棕榈酸Palmitic acid	—	0.22	—
57	（1R，4R，5S） -1，8-二甲基-4- （1-甲基乙烯基） -螺[4.5]癸-7-烯（1R，4R，5S）-1，8-dimethyl-4-（prop-1-en-2-yl）spiro[4.5]dec-7-ene	—	—	0.32
58	1，4，5-三甲基萘1，4，5-Trimethylnaphthalene	—	—	0.07
59	肉豆蔻酸异丙酯Isopropyl myristate	—	—	0.21

Table 5

Table 6

Fig.2

Table 7

Fig.3

References 0

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水平 Level	A 蒸气量 Vapor volume / （g·h^?1）	B 过热水蒸气温度 Temperature of superheated water vapor /℃	C 升温速度 Heating rate / （℃·min^?1）
1	600	310	1
2	800	320	2
3	1000	330	3

序号 Order number	A 蒸气量 Vapor volume / （g·h^?1）	B 过热水蒸气温度 Temperature of superheated water vapor /℃	C升温速度 Heating rate / （℃·min^?1）	烟熏香料得率 Yield of smoke flavorings （%）
1	600	310	1	25.98
2	600	320	3	25.12
3	600	330	2	24.76
4	800	310	3	27.07
5	800	320	2	28.05
6	800	330	1	28.74
7	1000	310	2	28.96
8	1000	320	1	29.70
9	1000	330	3	27.99
K₁	75.86	82.01	84.42	—
K₂	83.86	82.87	81.77	—
K₃	86.65	81.49	80.18	—
k₁	25.29	27.34	28.14	—
k₂	27.95	27.62	27.26	—
k₃	28.88	27.16	26.73	—
R	3.59	0.46	1.41	—

方差来源 Variance source	偏差平方和 Sum of squared deviations	自由度 Degree of freedom	均方 Mean square	F值 F-value	P值 P-value	显著性 Significance
蒸气量Vapor volume	20.912	2	10.456	73.975	0.013	*
过热水蒸气温度Temperature of superheated water vapor	0.324	2	0.162	1.146	0.466	—
升温速度Heating rate	3.059	2	1.529	10.820	0.085	—
误差Error	0.283	2	0.141

方法 Methods	得率 Yields（%）
水蒸气蒸馏法Steam distillation	0.76
干馏法Cracking process	6.94
过热水蒸气蒸馏?干馏法 Superheated steam distillation-cracking process integrated technology	29.45

名称 Name	相对质量分数Relative mass fraction（% ）
名称 Name	水蒸气蒸馏 SD	干馏 CP	过热水蒸气蒸馏? 干馏法SSD-CP
醇类化合物 Alcohol compounds	77.04	33.52	26.44
烯烃类化合物 Alkenes compounds	17.77	47.66	57.05
酯类化合物 Ester compounds	3.79	0.06	0.41
酚类化合物 Phenol compounds	—	15.19	14.48

Preparation of Smoke Flavorings of Cunninghamia lanceolata by Superheated Steam Distillation-Cracking and their Composition Analysis

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香料制备方法 Preparation method of flavorings	综合评价 Comprehensive evaluation
水蒸气蒸馏法 Steam distillation	清香、木香为主，整体香气纯正 The overall aroma is mainly characterized by a fresh and delicate fragrance with woody notes. It is pure and natural.
干馏法 Cracking process	焦甜香、木香为主，焦糊味严重，整体香气较沉闷 The aroma mainly comprises caramel and woody flavors, with a strong burnt taste and a dull overall fragrance.
过热水蒸气蒸馏?干馏法 Superheated steam distillation-cracking process integrated technology	焦甜香、木香为主，一点凉感，整体香气较通透持久 The aroma mainly comprises caramel and woody flavors， with a subtle cooling sensation， featuring overall transparency and long-lasting aroma.

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