CN103630658A - Method for identifying natural agilawood and artificial agilawood - Google Patents
Method for identifying natural agilawood and artificial agilawood Download PDFInfo
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- CN103630658A CN103630658A CN201310548720.7A CN201310548720A CN103630658A CN 103630658 A CN103630658 A CN 103630658A CN 201310548720 A CN201310548720 A CN 201310548720A CN 103630658 A CN103630658 A CN 103630658A
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Abstract
The invention discloses a method for identifying natural agilawood and artificial agilawood. The method is used for identifying natural agilawood and artificial agilawood by detecting the ratio of the content of chromone substances to the content of sesquiterpenoids substances in agilawood with a gas chromatography-mass spectrometer (GC-MS). When the ratio of the content of chromone substances and the content of sesquiterpenoids substances is less than 1, the agilawood is determined to be natural agilawood; when the ratio is more than 1, the agilawood is determined to be artificial agilawood; the quality of the artificial agilawood is higher when the ratio is closer to 1. Due to the adoption of the method for identifying natural agilawood and artificial agilawood, the natural agilawood and the artificial agilawood with different quality are distinguished so as to prompt the ordered and healthy development of the agilawood market, guarantee the benefit of widespread consumers and serve agilawood production and management enterprises.
Description
Technical field:
The invention belongs to biological technical field, be specifically related to a kind of method of differentiating natural agalloch eaglewood and artificial agalloch eaglewood.
Background technology:
Agalloch eaglewood (Aquilaria Resin, Aloeswood, Agarwood or Eaglewood) is to have traditional rare medicinal herbs of long applicating history and famous and precious natural perfume material, timber.The long history that agalloch eaglewood is used as medicine, has the history of 3000 at least at China and Japan.In < < Compendium of Materia Medica > >, recording agalloch eaglewood can " control heat in the upper and cold in the lower, the circulation of vital energy in the wrong direction be breathed heavily urgency, and large intestine void is closed, and urine gas drenches, man's cold sperm ".Agalloch eaglewood property is pungent, tepor, nontoxic, there is the effects such as promoting the circulation of qi analgesia, warming middle energizer to arrest vomiting, promoting inspiration to relieve asthma, for treatment abdominal distension, stomach cold, the obvious curative effects of suffering from a deficiency of the kidney, panted, since ancient times, agalloch eaglewood is processed to traditional Chinese medicine medicine materical crude slice conventionally, agalloch eaglewood is the prescription raw material of more than 160 Chinese patent drug at present, in the basic Chinese patent drug > > of < < China, uses the Chinese patent drug of agalloch eaglewood to reach 47 kinds.Traditional rare spice of agalloch eaglewood or a kind of and widespread use very popular in Asia.Most of agalloch eaglewoods almost can't smell fragrance under normal conditions, when smouldering, give off a strong fragrance, and can cover other smell, and fragrance remaining time is very long, are the high-grade spices of manufacturing essential oil and natural perfume.Agalloch eaglewood is one of Sapporo of enshrining and worship of Buddhism, and symbol Nazarite holds the perfume (or spice) of guarding against quietness, also can be described as the fragrance of extricator's soul, is used as the keeping spices of Buddhist portion.Agalloch eaglewood results from Thymelaeceae (Thymelaeaceae) plant, can produce approximately 32 of the seeds of agalloch eaglewood, and wherein agalloch eaglewood belongs to (Aquilaria) 25, intends agalloch eaglewood and belongs to (Gyrinops) 7.Suspension culture of Aquilaria sinensis (Aquila ria sinensis (Lour.) Gilg) mainly be take as main in China, have another name called buta-buta, for the torrid zone and subtropical evergreen arbor, it is unique plant resources that China produces agalloch eaglewood, being distributed in the ground such as Guangdong, Guangxi, Hainan, Taiwan and Yunnan of China, is also one of Guangdong genunie medicinal materials " ten large wide medicines ".
Agallochum is normal growth under field conditions (factors), and wooden white is comparatively soft, there is no fragrance, do not produce resin, at nature, agallochum is because be subject to after worm ant, the infringement naturally such as sick and wounded can secretion resin, and infiltrates, is deposited in xylem, and through for many years, knot is poly-forms, the age of tree is longer, face cream deposition is more of a specified duration, and agalloch eaglewood quality is better, and these are present in nature, the agalloch eaglewood that not human-induced produces, is referred to as natural agalloch eaglewood.According to wound, can stimulate the experience of agallochum secretion resin, in order to obtain more agalloch eaglewood, Shannon adopts the artificial methods such as the method for chopping wound, half disconnected bar method, the method that holes, baked wheaten cake method to stimulate suspension culture of Aquilaria sinensis tree, generally can cause Edgeworthia chrysantha.At present, by scientific research, find, the Edgeworthia chrysantha method of utilizing physics, chemistry and inoculated fungi all can produce agalloch eaglewood more or less around getting into the cave, existing a plurality of patents disclose the technical method that artificial induction agalloch eaglewood produces, as the agalloch eaglewood of CN 200710110082(cultivation), CN 201110184345(artificial induction's suspension culture of Aquilaria sinensis produces the method for agalloch eaglewood), CN 201010104119(transfusion is produced agalloch eaglewood on suspension culture of Aquilaria sinensis tree) etc.By these methods, can obtain a large amount of artificial agalloch eaglewood.
Natural agalloch eaglewood, it is general that because integration time is longer, often quality is better, but output is less.And manually agalloch eaglewood is because the Edgeworthia chrysantha time is short, often the more natural agalloch eaglewood of quality is poor for the reasons such as Edgeworthia chrysantha method divergence, but output is more, so on market, has occurred pretending to be with artificial agalloch eaglewood the phenomenon of natural agalloch eaglewood, to consumer, has brought loss.The simultaneously artificial quality of agalloch eaglewood own is uneven, lacks at present effective discriminating means, and market grading, transaction, management are all comparatively chaotic.We study discovery, and the agalloch eaglewood that natural agalloch eaglewood and artificial induction form has obvious difference on becoming to be grouped into, and it is better to approach the artificial agalloch eaglewood quality of natural agalloch eaglewood.This patent, by the discrimination method of natural agalloch eaglewood with artificial agalloch eaglewood is provided, makes a distinction the artificial agalloch eaglewood of natural agalloch eaglewood and different quality, and the Ordered and Healthy development for agalloch eaglewood market, guarantees consumers in general's interests, the production and operation enterprise of service agalloch eaglewood.
Summary of the invention:
The object of this invention is to provide a kind of method of differentiating the natural agalloch eaglewood forming under natural condition and the artificial agalloch eaglewood producing through artificial induction, utilize this method the artificial agalloch eaglewood of natural agalloch eaglewood and different quality can be made a distinction.
The present invention is the ratio situation with artificial agalloch eaglewood chromone class content of material and sesquiterpenoids content of material by more natural agalloch eaglewood, finds that both have obvious difference, and natural agalloch eaglewood ratio is less, and ratio is larger for artificial agalloch eaglewood.By above-mentioned discovery, realize the present invention.
The method of the natural agalloch eaglewood of discriminating of the present invention and artificial agalloch eaglewood, to differentiate natural agalloch eaglewood and artificial agalloch eaglewood by the ratio of chromone class content of material and sesquiterpenoids content of material in mensuration agalloch eaglewood, as the chromone class content of material by gas chromatography-mass spectrography (GC-MS) instrument mensuration agalloch eaglewood and the ratio of sesquiterpenoids content of material (mass percent).When the ratio of chromone class content of material and sesquiterpenoids content of material is less than 1, this agalloch eaglewood can be defined as natural agalloch eaglewood; When ratio is greater than 1, think that it is artificial agalloch eaglewood, ratio more approaches 1, and artificial agalloch eaglewood quality is better.If do not contained this two constituents, be personation agalloch eaglewood or the sample of Edgeworthia chrysantha not.The method of the natural agalloch eaglewood of discriminating provided by the invention and artificial agalloch eaglewood, in mensuration agalloch eaglewood, chromone class content of material and sesquiterpenoids content of material are to be detected by gas chromatography-mass spectrography (GC-MS) instrument.The sample detecting for GC-MS can utilize solvent methenyl choloride, at ambient temperature, the agalloch eaglewood after pulverizing is extracted and is obtained for 24 hours.
Wherein, a series of compounds that the chromone derivative that look letones refers to contain 2-phenethyl (2-phenylethyl) is representative, include but not limited to 13-Docosen-1-ol, (Z)-; 6-methoxy-2-(2-phenylethyl) chromone; 5,8-dihy droxy-2-(2-phenylethyl) chromone; 6-hydroxy-2-(2-phenylethyl) chromone; 6,7-dimethoxy-2-[2-(3'-methoxyphenyl) ethyl] chromone; 5,8-dihydroxy-2-[2-(4'-methoxyphenyl) ethyl] chromone; Hydrastine; 6,7-dimethoxy-2-(2-phenylethyl) chromone.Sesquiterpenoids material refers to that take the sequiterpene natural terpenes compounds of 15 carbon atoms (in the molecule containing), as a series of compounds of representative, includes but not limited to (-)-Spathulenol; Acetate, (2,4a, 5,8a-tetramethyl-1,2,3,4,4a, 7,8,8a-octahydro-1-naphthalenyl) ester; Farnesol; 5,6,6-Trimethyl-5-(3-oxobut-1-enyl)-1-oxaspiro[2.5] octan-4-one; B-Selinenol; Aristolone; Ledene o xide-(I); Baimuxinal; Verrucarol; Glaucyl alcohol; Saussurea lactone, dehydro; Velleral; Pro panedioic acid, 2-[(4-morpholyl) (phenyl) methyl]-, dimethyl ester; 4-Benzyloxynitrobenzene.
When GC-MS measures, adopt Rtx-5MS quartz capillary chromatographic column, when column temperature is 230 ℃, look letones of the present invention refers to that retention index is all compounds between 2400 to 3400; Sesquiterpenoids material of the present invention refers to that retention index is all compounds between 1400 to 2000.Described sesquiterpenoids material and the retention index of the representative compound of look letones under above-mentioned chromatographic condition are listed in table 1.
Table 1: adopt Rtx-5MS quartz capillary chromatographic column, retention index corresponding to different compounds when column temperature is 230 ℃
The present invention is by measuring look letones in agalloch eaglewood and ratio with sesquiterpenoids content of material, can effectively distinguish the agalloch eaglewood of natural agalloch eaglewood and artificial Edgeworthia chrysantha, by the size of ratio, can infer the quality of artificial Edgeworthia chrysantha effect simultaneously, for the grade classification of artificial agalloch eaglewood provides foundation, promote the Ordered and Healthy development in agalloch eaglewood market, guarantee consumers in general's interests, the production and operation enterprise of service agalloch eaglewood.
Embodiment:
Following examples are to further illustrate of the present invention, rather than limitation of the present invention.
Embodiment 1:
10, the agalloch eaglewood sample of natural Edgeworthia chrysantha is collected in field, pulverizes (crossing 60 mesh sieves).Each sample is got 0.5g, accurately weighed, puts in tool plug conical flask, and precision adds methenyl choloride 10mL, and close plug shakes up, weighed weight, cold soaking 24h.Extract carries out evaporate to dryness in water-bath in 80 ℃, obtains medicinal extract, adds methenyl choloride and makes to dissolve, and quantitatively to 2mL, with filtering with microporous membrane (0.45 μ m), gets 1 μ L loading.Gas chromatograph-mass spectrometer (GCMS) chromatographic condition: chromatographic column is Rtx-5MS quartz capillary column; 230 ℃ of injector temperatures; Carrier gas is high-purity helium, flow velocity 1.0mL/min, and sample size is 1 μ L, 1:30 split sampling.Heating schedule: 90 ℃ of insulation 4min, 2.5 ℃/min is warming up to 160 ℃ of insulation 5min, and 0.3 ℃/min is warming up to 180 ℃ of insulation 5min, and 2 ℃/min is warming up to 200 ℃, and 1 ℃/min is warming up to 230 ℃ of insulation 120min.Mass spectrum condition is that ion gun is EI; Ionizing energy 70ev; Ionization voltage 1977mV, 171 ℃ of ion temperatures, solvent time delay 4min; Mass scanning scope 50～550m/z.
By Shimadzu chem workstation (V2.0), identify in application Wiley138 mass spectrometric data storehouse, and adopt areas of peak normalization method to calculate retention index to be that all compounds (look letones) and retention index between 2400 to 3400 is the ratio of the content of all compounds (sesquiterpenoids material) between 1400 to 2000, to the results are shown in Table 2.
Result demonstration, the ratio of the look letones of natural agalloch eaglewood and the content of sesquiterpenoids material is between 0.290-0.663.
Table 2: the look letones in natural agalloch eaglewood and the ratio of sesquiterpenoids content of material
Embodiment 2:
Get by formic acid and induce 10, the agalloch eaglewood sample that produces, the assay method of look letones and sesquiterpenoids content of material ratio, with embodiment 1, the results are shown in Table 3.
Result demonstration, the ratio that formic acid induction produces the look letones of agalloch eaglewood and the content of sesquiterpenoids material is between 1.095-8.840.
Table 3: formic acid induction produces the look letones of agalloch eaglewood and the ratio of sesquiterpenoids content of material
Embodiment 3:
Get by microbial inoculum and induce 10, the agalloch eaglewood sample that produces, the assay method of look letones and sesquiterpenoids content of material ratio, with embodiment 1, the results are shown in Table 4.
Result demonstration, the ratio that microbial inoculum induction produces the look letones of agalloch eaglewood and the content of sesquiterpenoids material is between 1.550-10.546.
Table 4: microbial inoculum induction produces the look letones of agalloch eaglewood and the ratio of sesquiterpenoids content of material
Claims (7)
1. a method of differentiating natural agalloch eaglewood and artificial agalloch eaglewood, it is characterized in that, by measuring chromone class content of material in agalloch eaglewood, differentiate natural agalloch eaglewood and artificial agalloch eaglewood with the ratio of sesquiterpenoids content of material, ratio be less than 1 be natural agalloch eaglewood, ratio be greater than 1 be artificial agalloch eaglewood.
2. the method for the natural agalloch eaglewood of discriminating according to claim 1 and artificial agalloch eaglewood, is characterized in that, in described agalloch eaglewood, chromone class content of material and sesquiterpenoids content of material are to be measured by gas chromatograph-mass spectrometer (GCMS).
3. assay method according to claim 2, is characterized in that, the sample that described gas chromatograph-mass spectrometer (GCMS) is measured is to utilize solvent methenyl choloride, at ambient temperature, the agalloch eaglewood after pulverizing is extracted and is obtained for 24 hours.
4. the method for the natural agalloch eaglewood of discriminating according to claim 1 and artificial agalloch eaglewood, is characterized in that, described look letones comprises 13-Docosen-1-ol, (Z)-; 6-methoxy-2-(2-phenylethyl) chromone; 5,8-dihydroxy-2-(2-phenylethyl) chromone; 6-hydroxy-2-(2-phenylethyl) chromone; 6,7-dimethoxy-2-[2-(3'-m ethoxyphenyl) ethyl] chromone; 5,8-dihydroxy-2-[2-(4'-methoxyphenyl) ethyl] chromone; Hydrastine; 6,7-dimethoxy-2-(2-phenylethyl) chromone.
5. the natural agalloch eaglewood of discriminating according to claim 1 and the manually method of agalloch eaglewood, it is characterized in that, described look letones is for adopting Rtx-5MS quartz capillary chromatographic column, column temperature is under the condition of 230 ℃, while carrying out gas chromatography-mass spectrography mensuration, retention index is all compounds between 2400 to 3400.
6. the method for the natural agalloch eaglewood of discriminating according to claim 1 and artificial agalloch eaglewood, is characterized in that, described sesquiterpenoids material comprises (-)-Spathulenol; Acetate, (2,4a, 5,8a-tetramethyl-1,2,3,4,4a, 7,8,8a-octahydro-1-na phthalenyl) ester; Farnesol; 5,6,6-Trimethyl-5-(3-oxobut-1-enyl)-1-oxaspiro[2.5] octan-4-one; B-Selinenol; Aristolone; Ledene oxide-(I); Baimuxinal; Verrucarol; Glaucyl alcohol; Sa ussurea lactone, dehydro; Velleral; Propanedioic acid, 2-[(4-morpholyl) (phenyl) methyl]-, dimethyl ester; 4-Benzyloxynitrobenzene.
7. the natural agalloch eaglewood of discriminating according to claim 1 and the manually method of agalloch eaglewood, it is characterized in that, described sesquiterpenoids material is for adopting Rtx-5MS quartz capillary chromatographic column, column temperature is under the condition of 230 ℃, while carrying out gas chromatography-mass spectrography mensuration, retention index is all compounds between 1400 to 2000.
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| CN105699343A (en) * | 2016-01-05 | 2016-06-22 | 华南农业大学 | Method for nondestructively identifying authenticity of agilawood |
| CN106053645A (en) * | 2016-06-01 | 2016-10-26 | 中国广州分析测试中心 | Method for identifying authenticity of agilawood |
| CN106198791A (en) * | 2016-06-28 | 2016-12-07 | 中山出入境检验检疫局检验检疫技术中心 | Lignum Aquilariae Resinatum tetrol and the method for benzylacetone in a kind of Lignum Aquilariae Resinatum of mensuration simultaneously |
| CN106290613A (en) * | 2016-07-28 | 2017-01-04 | 中国热带农业科学院热带生物技术研究所 | A kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false |
| CN107271594A (en) * | 2017-07-14 | 2017-10-20 | 河南中大恒源生物科技股份有限公司 | A kind of method for differentiating Natural Curcumin and synthesis curcumin |
| CN108802253A (en) * | 2017-12-11 | 2018-11-13 | 北京林业大学 | A kind of discrimination method of strange nanmu agalloch eaglewood and the common agalloch eaglewood of Huian system |
| CN108802252A (en) * | 2017-12-11 | 2018-11-13 | 北京林业大学 | A kind of discriminating star continent system agalloch eaglewood and Huian system agalloch eaglewood class method for distinguishing |
| CN109406679A (en) * | 2018-12-11 | 2019-03-01 | 北京三和药业有限公司 | A kind of detection method of high effective liquid chromatography for measuring agalloch eaglewood quality |
| CN110221012A (en) * | 2019-06-03 | 2019-09-10 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of construction method of agalloch eaglewood digitlization Chromatography/Mass Spectrometry finger-print |
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| CN105699343B (en) * | 2016-01-05 | 2018-08-14 | 华南农业大学 | A kind of method of agalloch eaglewood true and false Undamaged determination |
| CN105699343A (en) * | 2016-01-05 | 2016-06-22 | 华南农业大学 | Method for nondestructively identifying authenticity of agilawood |
| CN106053645B (en) * | 2016-06-01 | 2019-04-05 | 中国广州分析测试中心 | A method of identifying the agalloch eaglewood true and false |
| CN106053645A (en) * | 2016-06-01 | 2016-10-26 | 中国广州分析测试中心 | Method for identifying authenticity of agilawood |
| CN106198791A (en) * | 2016-06-28 | 2016-12-07 | 中山出入境检验检疫局检验检疫技术中心 | Lignum Aquilariae Resinatum tetrol and the method for benzylacetone in a kind of Lignum Aquilariae Resinatum of mensuration simultaneously |
| CN106198791B (en) * | 2016-06-28 | 2018-09-11 | 中山出入境检验检疫局检验检疫技术中心 | Method that is a kind of while measuring agalloch eaglewood tetrol and benzylacetone in agalloch eaglewood |
| CN106290613A (en) * | 2016-07-28 | 2017-01-04 | 中国热带农业科学院热带生物技术研究所 | A kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false |
| CN106290613B (en) * | 2016-07-28 | 2019-06-07 | 中国热带农业科学院热带生物技术研究所 | A method of identifying the odd nanmu agalloch eaglewood true and false |
| CN107271594A (en) * | 2017-07-14 | 2017-10-20 | 河南中大恒源生物科技股份有限公司 | A kind of method for differentiating Natural Curcumin and synthesis curcumin |
| CN108802252A (en) * | 2017-12-11 | 2018-11-13 | 北京林业大学 | A kind of discriminating star continent system agalloch eaglewood and Huian system agalloch eaglewood class method for distinguishing |
| CN108802253A (en) * | 2017-12-11 | 2018-11-13 | 北京林业大学 | A kind of discrimination method of strange nanmu agalloch eaglewood and the common agalloch eaglewood of Huian system |
| CN108802253B (en) * | 2017-12-11 | 2020-07-07 | 北京林业大学 | Identification method of Kyara and Huian common agilawood |
| CN108802252B (en) * | 2017-12-11 | 2020-07-07 | 北京林业大学 | Method for identifying categories of star continent series agilawood and Huian series agilawood |
| CN109406679A (en) * | 2018-12-11 | 2019-03-01 | 北京三和药业有限公司 | A kind of detection method of high effective liquid chromatography for measuring agalloch eaglewood quality |
| CN110221012A (en) * | 2019-06-03 | 2019-09-10 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of construction method of agalloch eaglewood digitlization Chromatography/Mass Spectrometry finger-print |
| CN110221012B (en) * | 2019-06-03 | 2021-03-26 | 广东省测试分析研究所（中国广州分析测试中心） | Method for constructing digital chromatography/mass spectrum fingerprint of agilawood |
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