CN104830528A - Preparation method and use method of aquilaria wood perfume - Google Patents

Preparation method and use method of aquilaria wood perfume Download PDF

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Publication number
CN104830528A
CN104830528A CN201510196176.3A CN201510196176A CN104830528A CN 104830528 A CN104830528 A CN 104830528A CN 201510196176 A CN201510196176 A CN 201510196176A CN 104830528 A CN104830528 A CN 104830528A
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China
Prior art keywords
agalloch eaglewood
preparation
spices
perfume
aquilaria wood
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CN201510196176.3A
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CN104830528B (en
Inventor
吴新星
余汉谋
姜兴涛
李剑政
肖海鸿
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Botton Spices Co ltd
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Dongguan Bowden Spices Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes

Abstract

The invention relates to the technical field of perfume and especially relates to a preparation method and use method of aquilaria wood perfume. The preparation method comprises putting aquilaria wood chips into a glass container with an upper opening, adding a stainless steel theta net ring filler into the glass container, connecting a condensation reflux device to the upper end of the glass container, heating the bottom of the glass container with the aquilaria wood chips, collecting aromatic compound distillate by the condensation reflux device connected to the upper end of the glass container, dissolving the collected aromatic compound distillate in anhydrous ethanol, carrying out refrigeration treatment on the solution, carrying out filtration, and carrying out reduced pressure condensation to obtain the aquilaria wood perfume. The aquilaria wood perfume has a fragrance the same as that of aquilaria wood champignon. The preparation method has simple processes and high productivity and is suitable for industrial production. The aquilaria wood perfume is economic and practical and can be used in the field of daily chemical flavor adjustment and champignon. The aquilaria wood perfume is arranged in a room and produces a fragrance by supersonic wave atomization thereby producing tranquilizing and excitement allaying effects.

Description

A kind of preparation method of agalloch eaglewood spices and using method
Technical field
The present invention relates to spices technical field, particularly relate to a kind of preparation method and using method of agalloch eaglewood spices.
Background technology
Agalloch eaglewood is the resiniferous timber of thymelaeceae eaglewood Lignum Aquilariae Resinatum Aquilaria sinensis, and being the kind that " Chinese Pharmacopoeia " records, is the QI regulating medicine commonly used clinically.Agalloch eaglewood is a kind of traditional rare medicinal herbs and natural perfume, has sending down abnormally ascending, Wen Zhong, warms up the supporing yang function of kidney.Cure mainly the vexed pain of chest abdominal distension, gastrofrigid vomiting hiccup, the circulation of vital energy in the wrong direction of suffering from a deficiency of the kidney breathe heavily urgency.Agalloch eaglewood is higher containing the amount of volatile oil, and having strong fragrance, is the main component of agalloch eaglewood volatility drug effect, and its amount containing volatile oil is directly relevant to the quality of medicinal material.
The preparation method of current agalloch eaglewood spices comprises steam distillation, supercritical fluid extraction, solvent extration, subcritical abstraction method etc., but the fragrance difference that the agalloch eaglewood spices prepared of these methods and agalloch eaglewood champignon produce is very large.And agalloch eaglewood of directly burning produces naked light, easily cause security incident.How preparing the agalloch eaglewood spices consistent with fragrance during agalloch eaglewood champignon is central point of the present invention.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method and using method of agalloch eaglewood spices, and it is simple that it has preparation method, and be conducive to suitability for industrialized production, the spices fragrance of preparation is pure.
For achieving the above object, the technical solution used in the present invention is as follows:
A preparation method for agalloch eaglewood spices, comprises the following steps:
A. by agalloch eaglewood wood chip and the mixing of stainless steel Dixon ring filler, be positioned in the Glass Containers of a upper end open;
B. the external condensation reflux unit in Glass Containers upper end;
C. to the Glass Containers bottom-heated being mounted with agalloch eaglewood wood chip, the external condensation reflux unit in Glass Containers upper end is utilized to collect the aromatic compound distilled;
D. add anhydrous alcohol solution by collecting the aromatic compound obtained, solute is after freezing treatment, and filter, concentrating under reduced pressure, obtains a kind of agalloch eaglewood spices.
Preferably, described in step a, agalloch eaglewood wood chip granularity is 3 ~ 8mm.Agalloch eaglewood wood chip granularity is unsuitable excessive, agalloch eaglewood wood chip accumulation granularity is too large, be unfavorable for that agalloch eaglewood carries out aerobic cracking, produce aromatic compound, add stainless steel Dixon ring filler, the space between agalloch eaglewood wood chip can be ensured further, thus promote aerobic cracking, also ensure the thermally equivalent of agalloch eaglewood wood chip simultaneously, avoid coking.
Preferably, stainless steel Dixon ring filler addition described in step a is agalloch eaglewood bits 2 ~ 5 times of weight, and load that total height is no more than Glass Containers 2/5ths.Stainless steel Dixon ring filler, also known as Dixon (Dixon) filler, is a kind of efficient packing of small particle, makes with wire cloth, and the diameter of filler is with highly equal.Due to the wicking action of wire cloth, liquid can disperse film forming well, is beneficial to gas-liquid two and carries out abundant mass transfer, heat transfer, significantly can eliminate the wild effects such as channel.
Preferably, type of heating described in step c is common electrically heated or microwave heating, and heating rate is 5 DEG C/min, when being heated to preset temperature, keeps 20 ~ 40min.Slow heating is conducive to the progressively aerobic cracking of agalloch eaglewood wood chip.
Preferably, the top temperature of described preset temperature is 250 DEG C ~ 280 DEG C.At this temperature, distillation can collect target distillation material, and ensure that agalloch eaglewood wood chip does not produce pyrogenic reaction, affects the quality of final spices.
Preferably, adding dehydrated alcohol amount described in steps d is 3 ~ 5 times that collect the aromatic compound weight obtained.So, can ensure that aromatic compound is fully dissolved in dehydrated alcohol, and have enough amount of solution circulation distillations, while guarantee obtains target distillation material, improve productive rate.
Preferably, the freezing treatment time described in steps d is 24h ~ 36h.After freezing treatment, filter the insoluble wax in removal aromatic compound and impurity component, ensure that the aroma component of final spice product.
Preferably, the temperature of concentrating under reduced pressure described in steps d is 45 DEG C ~ 55 DEG C, and pressure is-0.08 ~-0.09MPa.
Preferably, described Glass Containers is glass round bottom container.Be heated evenly during the heating of glass round bottom container, heating surface area is large, is convenient to backflow and the volatilization of steam, is conducive to enhancing productivity.
The using method of above-mentioned a kind of agalloch eaglewood spices is: the agalloch eaglewood spices prepared is placed in ultrasonic atomizer and evaporates by steaming smoked mode, ultrasonic frequency is 1.7MHz ± 0.17MHz.Without the need to burning, spices produces champignon, avoids the possibility of naked light security incident.
Beneficial effect of the present invention is: the agalloch eaglewood spices prepared by the present invention is consistent with the fragrance of agalloch eaglewood champignon, and preparation method's easy handling, productivity is high, is suitable for suitability for industrialized production, be a kind of more economic and practical agalloch eaglewood spices, can be applicable to daily use chemicals blending and champignon field.Obtained agalloch eaglewood spices is positioned over indoor, is evaporated by means such as ultrasonic atomizations, thus reach calm effect of calming the nerves.
Accompanying drawing explanation
Utilize accompanying drawing to be described further invention, but the embodiment in accompanying drawing does not form any limitation of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to the following drawings.
Fig. 1 is the gas chromatogram of the agalloch eaglewood spices that the present invention obtains.
Embodiment
embodiment 1
The preparation method of a kind of agalloch eaglewood spices of the present embodiment, comprises the following steps:
A. 100g eaglewood powder is broken to the agalloch eaglewood wood chip that granularity is 5mm, mixes with 200g stainless steel Dixon ring filler, be positioned in the glass round bottom container of a upper end open;
B. the external condensation reflux unit in Glass Containers upper end;
C. to the glass round bottom container bottom heating being mounted with agalloch eaglewood wood chip, with the heating rate of 5 DEG C/min, when Heating temperature reaches 250 DEG C, keep 30min, the external condensation reflux unit of glass round bottom container upper end is utilized to collect the aromatic compound distilled, 0.85g;
D. add 3.4g anhydrous alcohol solution by collecting the aromatic compound obtained, solute is through freezing treatment 36h, and filter, at 50 DEG C, concentrating under reduced pressure under-0.09MPa condition, obtains 0.6g oily agalloch eaglewood spices.
Productive rate=0.6g/100g × the 100%=6 ‰ of agalloch eaglewood spices.
embodiment 2-4
The preparation process of embodiment 2-4 is identical with embodiment 1, and preparation parameter is as shown in table 1.
Table 1
Respectively the agalloch eaglewood spices obtained by embodiment 1 to 4 is placed in ultrasonic atomizer to evaporate by steaming smoked mode, ultrasonic frequency is 1.7MHz ± 0.17MHz.The fragrance distributed is consistent with the fragrance of agalloch eaglewood champignon, plays calm effect of calming the nerves, and produces champignon, use safety without the need to the spices that burns.
The volatile and semi-volatile compounds of obtained agalloch eaglewood spices is detected by gas chromatography-mass spectrum, its chemical composition identified and mass fractions relative as shown in table 2, gas chromatogram is as shown in Figure 1.GC conditions: chromatographic column: Agilent 19091S-105(50.0m × 0.2mm × 0.33 μm); Temperature programming: initial temperature 50 DEG C, 2 DEG C/min temperature programming to 150 DEG C, 4 DEG C/min temperature programming to 270 DEG C, retains 10min; Injector temperature: 250 DEG C; Carrier gas is helium (mass component); Carrier gas flux: constant 1.0mL/min; Splitting ratio: 40:1, sample size: 0.6uL; Adopt area normalization standard measure.
Table 2
No. Retention time/min Compound Mass fractions relative/%
1 3.570 Formic acid 0.591
2 4.105 Acetic acid 4.285
3 4.220 Propionic acid 0.360
4 4.701 Pyruvic alcohol 0.163
5 4.932 Vinylformic acid 0.194
6 5.272 Hydroxy methyl acetate 0.101
7 5.816 Pyridine 0.128
8 6.446 Ethanamide 0.280
9 6.541 Diacetamide 0.472
10 7.916 2-butylene acid 0.191
11 9.055 Furfural 0.265
12 9.669 3-methyl-3-butenoic acid 0.225
13 9.832 Furfuryl alcohol 0.088
14 10.302 3-methyl-2-butenoic acid 0.259
15 10.512 Lactic acid 0.259
16 10.901 2-methyl-2-butenoic acid 0.025
17 11.059 Butyl cellosolve 0.086
18 11.525 2 (5H)-furanones 0.831
19 11.820 3-hydroxy-propionic acid 0.261
20 11.982 2-hydroxyl-2-cyclopentene-1-one 0.217
21 12.966 β-angelica lactone 0.105
22 13.790 5 methyl furfural 0.015
23 14.819 Phenol 0.175
24 15.124 3-furancarboxylic acid 0.300
25 15.536 2-hydroxy-gamma-butyrolactone 0.346
26 16.028 3-Methoxy Pyridine 0.078
27 16.576 N-formylpyrrole 0.054
28 16.709 Methyl cyclopentenyl ketone 1.007
29 16.967 4-methyl-2 (5H) furanone 0.110
30 17.557 Phenylcarbinol 0.119
31 17.769 Levulinic acid 0.227
32 20.127 Furanone 0.329
33 20.416 Methylfuroate 0.065
34 20.966 Furancarboxylic acid 1.225
35 21.240 Methyl catechol 0.177
36 22.844 Voitol 0.860
37 23.105 3-pyridone 0.550
38 24.176 Phenylformic acid 1.228
39 24.824 Hydration voitol 0.249
40 25.393 Single-ethyl succinate 0.172
41 27.504 Hydroxyl voitol 0.482
42 28.055 Pyrocatechol 0.577
43 28.470 To methyl guaiacol and 4 0.128
44 29.918 P methoxy phenol 0.407
45 30.619 5 hydroxymethyl furfural 4.240
46 30.835 Toluylic acid 0.404
47 31.686 Glucopyranose acetic ester 3.918
48 31.909 Anisyl aldehyde 0.761
49 32.425 3-methoxyl group pyrocatechol 0.368
50 33.057 Anisy alcohol 0.049
51 33.456 2-ethanoyl Resorcinol 0.109
52 33.935 Resorcinol 0.526
53 35.308 Salicylaldhyde 0.100
54 35.475 5 hydroxymethyl furfural acetic ester 0.520
55 36.024 To vinyl guaiacol 0.100
56 37.102 Tetra hydro Phthalic anhydride 0.050
57 37.465 Phenylpropionic acid 2.442
58 38.067 2,6-syringol 2.378
59 38.422 P-methoxy-acetophenone 0.095
60 38.597 Isoeugenol 0.091
61 39.194 P-Hydroxybenzaldehyde 0.728
62 41.187 Ortho-methylthio phenol 0.839
63 41.798 Cinnamic acid 0.088
64 42.428 Anisic acid 0.698
65 43.828 Different vanillinated 1.134
66 44.516 To propyl guaiacol 0.291
67 46.051 To ethanoyl methyl catechol 0.941
68 46.779 Anisylacetone 0.690
69 47.870 Vanillinated methyl esters 0.332
70 49.592 3-ethanoyl methyl catechol 0.192
71 50.262 To propionyl methyl catechol 0.071
72 51.671 4-Methoxyhydrocinnamic acid 0.846
73 52.697 3,4-dihydroxyl-5-methoxybenzaldehyde 0.135
74 53.921 6-methoxyl group Eugenol 0.134
75 55.872 Syringic aldehyde 11.297
76 56.181 3-hydroxyl-4-methoxyl group cinnamic acid 0.044
77 55.368 Zingiberone 0.822
78 56.870 2,5-dimethoxy-3,4-Dihydroxy benzaldehyde 0.129
79 59.455 4-hydroxyl-2-methoxyl group cinnamic aldehyde 2.501
80 59.566 To ethanoyl syringone 1.137
81 60.753 4-hydroxy 3-methoxybenzene propionic acid 0.371
82 61.522 Methyl syringate 0.912
83 63.914 3,5-dimethoxy-4 '-hydroxy-benzoic acid 0.710
84 71.469 3,5-dimethoxy-4 '-hydroxyl cinnamic aldehyde 1.923
Agalloch eaglewood spices prepared by the present invention, volatility and half volatile material composition identify 84 kinds of compounds altogether, be mainly the organic acid of low carbon chain, alcohols, ester class, phenols, the materials such as ketone, what wherein content was higher has syringic aldehyde (11.297%), acetic acid (4.285%), 5 hydroxymethyl furfural (4.24%), Glucopyranose acetic ester (3.918%), 4-hydroxyl-2-methoxyl group cinnamic aldehyde (2.501%), the agalloch eaglewood spices prepared has stayed the original aroma component of agalloch eaglewood, comprise furanone, furfural, phenylformic acid etc., the fragrance evaporated by the smoked mode of ultrasonic atomizer steaming is consistent with fragrance during agalloch eaglewood champignon.
Preparation method's easy handling of the present invention, productivity is high, can reach 4.2 ‰ ~ 6.7 ‰, be suitable for suitability for industrialized production, is a kind of more economic and practical agalloch eaglewood spices, can be applicable to daily use chemicals blending and champignon field.
Finally should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although done to explain to the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.

Claims (10)

1. a preparation method for agalloch eaglewood spices, is characterized in that: comprise the following steps:
Step a., by agalloch eaglewood wood chip and the mixing of stainless steel Dixon ring filler, is positioned in the Glass Containers of a upper end open;
The external condensation reflux unit in step b. Glass Containers upper end;
Step c, to the Glass Containers bottom-heated being mounted with agalloch eaglewood wood chip, utilizes the external condensation reflux unit in Glass Containers upper end to collect the aromatic compound distilled;
Steps d. add anhydrous alcohol solution by collecting the aromatic compound obtained, solute is after freezing treatment, and filter, concentrating under reduced pressure, obtains a kind of agalloch eaglewood spices.
2. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: described in step a, agalloch eaglewood wood chip granularity is 3 ~ 8mm.
3. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: stainless steel Dixon ring filler addition described in step a is agalloch eaglewood bits 2 ~ 5 times of weight, and load that total height is no more than Glass Containers 2/5ths.
4. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: type of heating described in step c is common electrically heated or microwave heating, and heating rate is 5 DEG C/min, is heated to preset temperature.
5. the preparation method of a kind of agalloch eaglewood spices according to claim 4, is characterized in that: the top temperature of described preset temperature is 250 DEG C ~ 280 DEG C, keeps 20 ~ 40min.
6. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: adding dehydrated alcohol amount described in steps d is 3 ~ 5 times that collect the aromatic compound weight obtained.
7. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: the freezing treatment time described in steps d is 24h ~ 36h.
8. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: the temperature of concentrating under reduced pressure described in steps d is 45 DEG C ~ 55 DEG C, and pressure is-0.08 ~-0.09MPa.
9. the preparation method of a kind of agalloch eaglewood spices according to claim 1, is characterized in that: described Glass Containers is glass round bottom container.
10. the using method of an agalloch eaglewood spices, it is characterized in that: the agalloch eaglewood spices that the preparation method of a kind of agalloch eaglewood spices in claim 1-9 described in any one obtains is placed in ultrasonic atomizer and evaporates by steaming smoked mode, ultrasonic frequency is 1.7MHz ± 0.17MHz.
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Address after: No. 8, Xixi Road, Liaobu Town, Dongguan City, Guangdong Province, 523000

Patentee after: Botton Spices Co.,Ltd.

Address before: 523000 first floor, Fortune Building, Liaobu Town, Dongguan City, Guangdong Province

Patentee before: DONGGUAN BOTON FLAVORS & FRAGRANCES Co.,Ltd.

CP03 Change of name, title or address