CN106290613A - A kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false - Google Patents
A kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false Download PDFInfo
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Abstract
The present invention relates to analytical chemistry field, specifically disclose a kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false.Testing sample is extracted by described method, it is thus achieved that extract, calculates grease extraction efficiency simultaneously；Extract obtains monomeric compound 2 [2 (4 the methoxyphenethyl)] percentage contents of chromone, the percentage contents of monomeric compound 2 (2 phenethyl) chromone and the percentage contents of monomeric compound 6,7 dimethoxy 2 (2 phenethyl) chromone in testing sample by chemical analysis method；Testing sample is accredited as strange nanmu Lignum Aquilariae Resinatum simultaneously when meeting standard given to this invention.The present invention, by the systematic study to strange nanmu Lignum Aquilariae Resinatum, uses the characteristic component data that chemical analysis method obtains, it is provided that a kind of scientific system ground judges the standard of the strange nanmu Lignum Aquilariae Resinatum true and false, it is possible to identifies the strange nanmu Lignum Aquilariae Resinatum true and false exactly, possesses feasibility.
Description
Technical field
The present invention relates to analytical chemistry field, a kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false.
Background technology
Lignum Aquilariae Resinatum is that thymelaeceae Lignum Aquilariae Resinatum belongs to (Aquilaria) plant timber with resin.Strange nanmu be in Lignum Aquilariae Resinatum tops and
Most precious kind, has another name called strange nanmu, Lignum Aquilariae Resinatum, gal nanmu, gal etc., and English name has Kanankoh, Kyara, Chi-Nan, Qi-Nan
Deng, because of its mysterious graceful fragrance and abundant fat content, market at prices is the most expensive.Plant is in domestic strange nanmu Lignum Aquilariae Resinatum source
Thymelaeceae Lignum Aquilariae Resinatum.
At present, the discriminating of strange nanmu Lignum Aquilariae Resinatum relies only on sense organ discriminating, does not has chemical discrimination method.According to Xie Zongwan " Chinese crude drug product
Kind discuss (middle volume) " to record strange nanmu appearance glossy smooth, oiliness weight, carves it with fingernail, as husky in cone picture, and oil overflows immediately, uses cutter
Scraping, can twist with the fingers and pinch pelletization, become cake, can distribute durable delicate fragrance, and mildly bitter flavor is spicy, and that chews sticks to one's teeth, and fire is fuel-displaced.And common Lignum Aquilariae Resinatum
Matter is hard, and carving picks it, as bamboo scraped by cutter.Strange nanmu and common Lignum Aquilariae Resinatum sense organ differentiate that difference is more apparent.But it is this by sense organ discriminating side
Method requires that surveyor has very rich experience, and range of application is smaller.
Owing to lacking science quality discrimination technology easily, and traditional sense organ differentiate cannot widespread adoption, cause
Lignum Aquilariae Resinatum quality on the market is uneven, and fake and forged commodity, phenomenon of adulterating ratio are more serious.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false so that described method
Means by analytical chemistry, it is possible to identify the true and false of strange nanmu Lignum Aquilariae Resinatum exactly.
For achieving the above object, the present invention provides following technical scheme:
A kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false, including:
Step 1, testing sample is extracted, it is thus achieved that extract, calculate grease extraction efficiency simultaneously；
Step 2, extract obtain monomeric compound 2-[2-(the 4-methoxybenzene of testing sample by chemical analysis method
Ethyl)] percentage contents of chromone, the percentage contents of monomeric compound 2-(2-phenethyl) chromone and monomeric compound
The percentage contents of 6,7-dimethoxy-2-(2-phenethyl) chromone；
Step 3, testing sample are accredited as strange nanmu Lignum Aquilariae Resinatum simultaneously when meeting following standard；
(1) testing sample oils and fats extracts yield and must not be less than 10%；
(2) in testing sample, the percentage contents of monomeric compound 2-[2-(4-methoxyphenethyl)] chromone must not be low
In 20%；
(3) in testing sample, the percentage contents of monomeric compound 2-(2-phenethyl) chromone must not be less than 15%；
(4) in same testing sample, the percentage contents of 2-[2-(4-methoxyphenethyl)] chromone is higher than 2-(2-benzene
Ethyl) percentage contents of chromone；
(5) in testing sample, the percentage contents of monomeric compound 6,7-dimethoxy-2-(2-phenethyl) chromone is not
Must be more than 10%.
Sense organ is generally relied on to differentiate for strange nanmu Lignum Aquilariae Resinatum, the problem not having the chemical discrimination method of scientific system, the present invention
By to proposing a set of analysis method scientifically identifying its true and false after the systematic Study of strange nanmu Lignum Aquilariae Resinatum.
Wherein, as preferably, described in be extracted as organic solvent extraction, surname extraction, carbon dioxide supercritical fluid extraction
Or vapor distillation extracts.Extract of the present invention all can be extracted by these several extracting method and obtain, and grease extraction efficiency
It is calculated by grease extraction efficiency=extract quality/testing sample quality * 100%.
It is further preferred that in organic solvent extraction scheme organic solvent include ethyl acetate, ether, ethanol, normal hexane,
Petroleum ether, chloroform, methanol, n-butyl alcohol, alkane, benzene, acetone.Additionally, described surname extraction can also select use acetic acid second
Ester, ether, ethanol, normal hexane, petroleum ether, chloroform, methanol, n-butyl alcohol, alkane, benzene, acetone and other organic solvent are extracted.
In certain specific embodiments of the invention, have employed carbon dioxide supercritical fluid extraction, vapor distillation
Extraction, ether supersound extraction, ethyl acetate surname extraction and ethanol Soxhlet extraction.Ether supersound extraction concrete scheme is as follows:
Testing sample adds ether solvent, testing sample quality (g): ethyl acetate volume (mL) is (concrete less than 1:1
May be selected to be 2.590g:10mL), ultrasonic 15-30min, filters to obtain subsequent filtrate, is repeated twice, merge all subsequent filtrates, treat ether
Volatilize, obtain oily ether extract.
Ethyl acetate surname extraction concrete scheme is as follows:
Testing sample adds ethyl acetate solvent, utilizes surname extraction equipment, is heated to 90 DEG C and extracts acquisition oily extraction
Thing, testing sample quality (g): ethyl acetate volume (mL) is less than 1:2 (concrete may be selected to be 1.650g:10mL).
Ethanol Soxhlet extraction concrete scheme is as follows:
Testing sample adds alcohol solvent, utilizes surname extraction equipment, is heated to 110 DEG C and extracts acquisition oil-like extracts,
Testing sample quality (g): ethanol volume (mL) is less than 1:2 (concrete may be selected to be 1.380g:10mL).
Carbon dioxide supercritical fluid extraction concrete scheme is as follows:
Take testing sample 0.405g, mix homogeneously with 2.00g kieselguhr, obtain sample to be analyzed；It is analysed to sample load
Extracting pond, void volume kieselguhr fills up.Pond will be extracted be connected with supercritical fluid extraction equipment, extract.Extraction conditions
For: static extracting time 10min, dynamic extraction time 60min, pressure 20MPa, temperature 50～70 DEG C, CO2Flow velocity 2L/min；
Entrainer flow 0.4mL/min.
It is as follows that vapor distillation extracts concrete scheme:
Testing sample adds water, 110 DEG C, utilizes extraction by steam distillation, testing sample quality (g): water volume
(mL) 0.708g:100mL is referred to.
The percentage of monomeric compound 2-[2-(4-the methoxyphenethyl)] chromone of testing sample of the present invention contains
Amount, the percentage contents of monomeric compound 2-(2-phenethyl) chromone and monomeric compound 6,7-dimethoxy-2-(2-benzene second
Base) percentage contents of chromone can be obtained by existing analysis method, such as gas chromatogram, gas chromatography-mass spectrography, gas
Phase chromatograph-flight time mass spectrum, fast pyrogenation-gas chromatography mass spectrometry, (ultra high efficiency/efficiently) liquid chromatograph, high speed adverse current chromatogram, (super
Efficiently/efficiently) liquid chromatograph mass spectrography, efficient liquid phase-flight time mass spectrum, supercritical fluid chromatography-mass spectrometry.Its
In, the structural formula of three kinds of monomeric compounds is as follows:
For above-mentioned various chemical analysis methods, The present invention gives the method being the most preferably more conducive to analyze detection,
I.e. gas chromatogram, gas chromatography-mass spectrography, gas chromatogram-flight time mass spectrum, high performance liquid chromatography, ultra high efficiency liquid phase color
Spectrum-mass spectrometry.
Wherein, gas phase bar in described gas chromatogram, gas chromatography-mass spectrography, gas chromatogram-flight time mass spectrum condition
Part is preferably as follows:
Chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane fused-silica capillary column；Heating schedule: column temperature
50 DEG C, it is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, be warming up to 170 DEG C with 2 DEG C/min, keep 10min, with 5 DEG C/min
It is warming up to 310 DEG C, keeps 5min.
More specifically, in described gas chromatogram, gas chromatography-mass spectrography condition, gas phase condition is preferably as follows:
Chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane fused-silica capillary column；Heating schedule: column temperature
50 DEG C, it is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, be warming up to 170 DEG C with 2 DEG C/min, keep 10min, with 5 DEG C/min
It is warming up to 310 DEG C, keeps 5min；Temperature of vaporization chamber 250 DEG C；Carrier gas is high-purity He；Carrier gas flux 1.0mL/min；Sample size
1.0-2.0 μ L, does not shunts, solvent delay time: 4.0-5.0min.
In described gas chromatogram-flight time mass spectrum, gas phase condition is preferably as follows:
Chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane fused-silica capillary column；Heating schedule: column temperature
50 DEG C, it is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, be warming up to 170 DEG C with 2 DEG C/min, keep 10min, with 5 DEG C/min
It is warming up to 310 DEG C, keeps 5min；Temperature of vaporization chamber 250 DEG C；Carrier gas is high-purity He；Carrier gas flux 1.0mL/min；Sample size 1.0
μ L, split ratio: 10:1, solvent delay time: 4.0min.
Described gas chromatography-mass spectrography, gas chromatogram-flight time mass spectrum, (ultra high efficiency/efficient) liquid chromatograph-matter
In spectrum combination, Mass Spectrometry Conditions one of is preferably as follows:
(1) ESI ion source；Collision gas is helium, 0.4L/min；Atomization drying gas is high pure nitrogen
(99.999%), 6.0L/min；Capillary voltage-4000V；End plate voltage 500V；Nebulizer pressure 15psi；Mass scanning model
Enclose m/z 70 to 2200；
(2) electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature 150 DEG C；Connect
Mouth temperature 280 DEG C；Scan pattern: full scan；Mass scan range m/z 55～500；
(3) electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature 150 DEG C；Connect
Mouth temperature 280 DEG C；Scan pattern: full scan；Resolution: 8000FWHM.
(ultra high efficiency/efficiently) liquid chromatograph mass spectrography preferably (1st) kind, gas chromatography-mass spectrography preferably (2nd)
Kind, gas chromatogram-flight time mass spectrum preferably (3rd) is planted.
In described (ultra high efficiency/efficient) liquid chromatograph, (ultra high efficiency/efficient) liquid chromatograph mass spectrography, liquid-phase condition is excellent
Select as follows:
Dionex-Acclaim 120 C18Chromatographic column, mobile phase A is acetonitrile, and Mobile phase B is 0.5% aqueous formic acid, washes
De-Gradient program: 0～60min, 25%～55%A, 60～80min, 55%～80%A, 80～90min, 80%～100%A,
90～95min, 100%A；Flow velocity 0.4mL min-1, detect wavelength 254nm.More specifically, Dionex-Acclaim 120 C18
Chromatographic column, mobile phase A is acetonitrile, and Mobile phase B is 0.5% aqueous formic acid, gradient program: 0～60min, 25%～
55%A, 60～80min, 55%～80%A, 80～90min, 80%～100%A, 90～95min, 100%A；Flow velocity 0.4mL
min-1, detect wavelength 254nm, column temperature 26～30 DEG C, sample size 5～20 μ L.
Apply authentication method of the present invention that known strange nanmu Lignum Aquilariae Resinatum and common Lignum Aquilariae Resinatum are identified, qualification result complete
Cause, show that authentication method of the present invention has accuracy and feasibility higher, strange nanmu Lignum Aquilariae Resinatum can be carried out system, divides objectively
Analysis is identified.
From above technical scheme, the present invention, by the systematic study to strange nanmu Lignum Aquilariae Resinatum, uses chemical analysis method to obtain
The characteristic component data obtained, it is provided that a kind of scientific system ground judges the standard of the strange nanmu Lignum Aquilariae Resinatum true and false, it is possible to identify strange nanmu exactly
The Lignum Aquilariae Resinatum true and false, possesses feasibility.
Detailed description of the invention
The invention discloses a kind of method identifying the strange nanmu Lignum Aquilariae Resinatum true and false, in those skilled in the art can use for reference herein
Hold, be suitably modified technological parameter and realize.Special needs to be pointed out is, all similar replacements and change are to those skilled in the art
For be apparent from, they are considered as being included in the present invention.The method of the invention is entered by preferred embodiment
Having gone description, method described herein substantially can be changed in without departing from present invention, spirit and scope by related personnel
Dynamic or suitable change and combination, realize and apply the technology of the present invention.
Below in conjunction with embodiment, the present invention is expanded on further.
Embodiment 1:
Instrument: Agilent company of U.S. HP7820 GC instrument, is equipped with automatic sampler, chem workstation；Beijing Sai Duolisi
Balance company limited BP221S ten thousand/electronic scale；Trade company of Lay Boke surname extraction instrument.
Reagent: Tianjin Chemical Reagents Factory No.1's ethyl acetate (AR)；World company of the U.S. (Tedia) produces methanol (chromatograph
Pure).
Consumptive material: 2mL sample injection bottle, 0.45 μm organic facies microporous filter membrane.
Testing sample describes: it is blackish green that outward appearance is yellowish-brown colour band, strip and curly, the most deep mixed yellowish-brown
Oils and fats band is distributed on it, and oils and fats bar third dimension is obvious；On abnormal smells from the patient, aromatic flavor is mellow, sweet with as Olibanum taste and Mel
Taste；In feel, quality is thick and heavy, and hands pinches the glutinous sense in surface substantially；State cut by cutter: easily rolling.This sample is reflected by Senior Expert sense organ
Fixed, unanimously it is accredited as strange nanmu.
The authenticity of testing sample includes following step:
(1) pre-treatment of sample: take a fritter sample from this sample, shredding and accurately weighing weight is 1.650g；
(2) sample adds the ethyl acetate solvent of 10mL, utilizes surname extraction equipment, be heated to 90 DEG C and obtain oily extraction
Thing, accurately weighing weight is 0.3155g；
(3) according to formula: oils and fats extracts yield=extract quality/sample mass * 100% and calculates this sample ether extraction
Oil yield is 24.35%；
(4) accurately weigh a small amount of extract, be configured to the solution that concentration is 1mg/mL, cross organic microporous filter membrane of 0.45 μm
To the sample injection bottle of 2mL, obtain need testing solution；The most accurately weigh a small amount of monomeric compound A 2-[2-(4-methoxybenzene second
Base)] chromone, monomeric compound B 2-(2-phenethyl) chromone and monomeric compound C 6,7-dimethoxy-2-(2-phenethyl)
Chromone, is configured to the solution that concentration is 1mg/mL respectively, and the 0.45 organic microporous filter membrane of μm excessively, to the sample injection bottle of 2mL, obtains monomer
Compound A solution, monomeric compound B solution and monomeric compound C solution；
(5) utilizing gas chromatograph, be analyzed need testing solution and three monomeric compound solution, running parameter is such as
Under:
Gas phase condition: chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane (30m × 0.25mm × 0.25 μm)
Fused-silica capillary column；Heating schedule: column temperature 50 DEG C, is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, with 2 DEG C/min liter
Temperature, to 170 DEG C, keeps 10min, is warming up to 310 DEG C with 5 DEG C/min, keeps 5min；Temperature of vaporization chamber 250 DEG C；Carrier gas is high-purity
He (99.999%)；Carrier gas flux 1.0mL/min；Sample size 1.0 μ L, does not shunts, solvent delay time: 5.0min.
(6) obtain chromatogram, utilize the retention time of two monomeric compounds that testing sample is identified, and use peak
Area normalization method calculates the percentage contents of these three monomeric compound in testing sample, and qualification result is shown in Table 1.
Table 1 GC identifies the result of three components
| Numbering | Retention time | Compound name | Molecular formula | Molecular weight | Percentage contents |
| 1 | 37.63 | 2-(2-phenethyl) chromone | C17H14O2 | 250 | 19.45% |
| 2 | 42.02 | 2-[2-(4-methoxyl group) phenethyl] chromone | C18H16O3 | 280 | 44.47% |
| 3 | 49.03 | 6,7-dimethoxy-2-(2-phenethyl) chromone | C19H18O4 | 310 | 3.12% |
This sample detects monomeric compound A:2-[2-(4-methoxyl group) phenethyl] chromone (44.47%), singulation
Compound B:2-(2-phenethyl) chromone (19.45%) and monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone
(3.12%).
(7) according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, testing sample is identified, specific as follows:
1. this sample ether extraction oil yield is 24.35%, and more than 10%, touch the mark setting；
2. gas chromatograph (GC) detects monomeric compound A:2-in this sample [2-(4-methoxyphenethyl)] chromone
Relative amount be 44.47%, meet index regulation must not be less than 20%；
3. gas chromatograph (GC) detects the relative amount of monomeric compound B:2-in this sample (2-phenethyl) chromone
Being 19.45%, meet index regulation must not be less than 15%；
4. this sample is detected by gas chromatograph (GC), monomeric compound A:2-[2-(4-methoxyphenethyl)] chromone
Relative amount higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone.
5. gas chromatograph (GC) detects monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) color in this sample
The percentage contents of ketone is 3.12%, and meet index regulation must not be higher than 10%.
(8) operations according to the instant invention code, this sample meets all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, and this sample is
Strange nanmu Lignum Aquilariae Resinatum.
(9) identical analysis method is utilized to identify for the sample of worm leakage Lignum Aquilariae Resinatum through expert testimony, this sample description:
Outward appearance: spreading yellowish-brown oils and fats in white wooden portion, there are two worm holes on surface；Abnormal smells from the patient: have light fragrance；Feel: quality is light,
Hands pinches surface without glutinous sense；State cut by cutter: be difficult to cutting.Identify according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, specific as follows:
1. this sample ether extraction oil yield is 3.28%, less than 10%, and the strangest nanmu index setting；
2. gas chromatograph (GC) detects monomeric compound A:2-in this sample [2-(4-methoxyphenethyl)] chromone
Relative amount be 0.25%, be unsatisfactory for index regulation must not be less than 20%；
3. gas chromatograph (GC) detects the relative amount of monomeric compound B:2-in this sample (2-phenethyl) chromone
Being 6.95%, be unsatisfactory for index regulation must not be less than 15%；
4. this sample is detected by gas chromatograph (GC), monomeric compound A:2-[2-(4-methoxyphenethyl)] chromone
Relative amount less than the relative amount of monomeric compound B:2-(2-phenethyl) chromone, be unsatisfactory for strange nanmu identification of indicator；
5. gas chromatograph (GC) detects monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) color in this sample
The percentage contents of ketone is 14.26%, and be unsatisfactory for index regulation must not be higher than 10%.
(10) operations according to the instant invention code, this sample is unsatisfactory for all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, this sample
Product are not strange nanmu Lignum Aquilariae Resinatum.
Embodiment 2:
Instrument: Dai An company of the U.S. and Brooker company of U.S. UPLC3000-MS combined instrument；Beijing Sai Duolisi balance has
Limit company BP221S ten thousand/electronic scale；U.S.'s Bransonic-5510E-DTH ultrasonic washing instrument.
Reagent: Tianjin Chemical Reagents Factory No.1's ether (AR)；World company of the U.S. (Tedia) produces methanol (chromatographically pure).
Consumptive material: 2mL sample injection bottle, 0.45 μm organic facies microporous filter membrane.
Testing sample describe: strip wood particle in appearance, surface is a little brown powdery, and seen from have dark brown oils and fats
Stria is distributed；On abnormal smells from the patient, fragrance is pure and fresh, simple and elegant；In feel, quality is general, and hands pinches surface without glutinous sense；State cut by cutter: can slightly become
Volume.This sample is identified by Senior Expert sense organ, is unanimously accredited as strange nanmu.
The authenticity of testing sample includes following step:
(1) pre-treatment of sample: take a fritter sample from this sample, shredding and accurately weighing weight is 2.590g；
(2) sample adds the ether solvent of 10mL, ultrasonic 20min, filters to obtain subsequent filtrate；Repeat this step twice, close
And subsequent filtrate, treat that it volatilizes, obtain oily ether extract, accurately weighing weight is 0.4587g；
(3) according to formula: oil yield=extract quality/sample mass * 100% calculates this sample ether extraction oils and fats
Yield is 17.71%；
(4) accurately weigh a small amount of extract, be configured to the solution that concentration is 1.2mg/mL, the filter membrane of mistake 0.45 μm to 2mL
Sample injection bottle, obtain need testing solution；
(5) utilizing Ultra Performance Liquid Chromatography-GC-MS, be analyzed need testing solution, running parameter is as follows:
Liquid-phase condition: Dionex-Acclaim 120 C18Chromatographic column (250mm × 4.6mm, 5 μm), flowing is acetonitrile mutually
(A) and 0.5% aqueous formic acid (B).Gradient program: 0～60min, 25%～55%A, 60～80min, 55%～
80%A, 80～90min, 80%～100%A, 90～95min, 100%A.Flow velocity 0.4mL min-1, detect wavelength 254nm, post
Temperature 26 DEG C, sample size 20 μ L.
Mass Spectrometry Conditions: ESI ion source；Collision gas is helium, 0.4L/min；Atomization drying gas is high pure nitrogen
(99.999%), 6.0L/min；Capillary voltage-4000V；End plate voltage 500V；Nebulizer pressure 15psi；Mass scanning model
Enclose m/z 70 to 2200.
(6) analysis obtains chromatogram and mass spectrum, and this sample component qualification result is shown in Table 2.
Table 2 UPLC-MS identifies the result of three components
This sample detects monomeric compound A:2-[2-(4-methoxyl group) phenethyl] chromone (47.85%), singulation
Compound B:2-(2-phenethyl) chromone (30.79%) and monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone
(2.19%).
(7) according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, testing sample is identified, specific as follows:
1. this sample ether extraction yield is 10.70%, and more than 10%, touch the mark setting；
2. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound A:2-[2-in this sample
(4-methoxyphenethyl)] relative amount of chromone is 47.85%, meet index regulation must not be less than 20%；
3. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound B:2-(2-benzene in this sample
Ethyl) relative amount of chromone is 30.79%, meet index regulation must not be less than 15%；
4. this sample is detected by Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS), monomeric compound A:2-[2-
(4-methoxyphenethyl)] relative amount of chromone is higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone.
5. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound C:6,7-bis-in this sample
The percentage contents of methoxyl group-2-(2-phenethyl) chromone is 2.19%, and meet index regulation must not be higher than 10%.
(8) operations according to the instant invention code, this sample meets all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity identification method, this sample
Product are strange nanmus.
(9) utilize identical analysis method to being that manually the burrow sample of Lignum Aquilariae Resinatum is identified through expert testimony, this sample
Describe: outward appearance: spreading brown oils and fats on yellow-white xylem, there is the hole of a diameter of 2.5cm side；Abnormal smells from the patient: distribute simple and elegant
Fragrance；Feel: quality is light, and hands pinches surface without glutinous sense；State cut by cutter: easily cut, not rolling.According to strange nanmu Lignum Aquilariae Resinatum identification of indicator
Identify, specific as follows:
1. this sample ether extraction yield is 3.58%, less than 10%, and the strangest nanmu Lignum Aquilariae Resinatum index setting；
2. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound A:2-[2-in this sample
(4-methoxyphenethyl)] relative amount of chromone is 1.38%, be unsatisfactory for index regulation must not be less than 20%；
3. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound B:2-(2-benzene in this sample
Ethyl) relative amount of chromone is 6.89%, be unsatisfactory for index regulation must not be less than 15%；
4. this sample is detected by Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS), monomeric compound A:2-[2-
(4-methoxyphenethyl)] relative amount of chromone is less than the relative amount of monomeric compound B:2-(2-phenethyl) chromone, no
Meet strange nanmu identification of indicator；
5. Ultra Performance Liquid Chromatography-GC-MS (UPLC-MS) detects monomeric compound C:6,7-bis-in this sample
The percentage contents of methoxyl group-2-(2-phenethyl) chromone is 5.19%, and meet index regulation must not be higher than 10%.
(10) operations according to the instant invention code, the most 4. this sample is unsatisfactory for the index of strange nanmu Lignum Aquilariae Resinatum authenticity,
This sample is not strange nanmu Lignum Aquilariae Resinatum.
Embodiment 3:
Instrument: Agilent company of U.S. HP6890/5975C GC/MS combined instrument, is equipped with automatic sampler, chemical work
Stand；Beijing Sai Duolisi balance company limited BP221S ten thousand/electronic scale；U.S.'s Bransonic-5510E-DTH ultrasound wave
Cleaning device, 200mL heating mantle, condensing tube, 200mL round-bottomed flask.
Reagent: world company of the U.S. (Tedia) produces methanol (chromatographically pure).
Consumptive material: 2mL sample injection bottle, 0.45 μm organic facies microporous filter membrane.
Testing sample describes: block wood particle in appearance, and surface is yellowish-brown, and seen from have yellowish-brown oils and fats stria to divide
Cloth；On abnormal smells from the patient, sweet taste is strong；In feel, quality is general, and hands pinches surface glutinous sense；State cut by cutter: can slightly rolling.This sample passes through
Senior Expert sense organ is identified, is unanimously accredited as strange nanmu.
The authenticity of testing sample includes following step:
(1) pre-treatment of sample: take a fritter sample from this, shredding and accurately weighing weight is 0.708g；
(2) sample adds 100mL water, 110 DEG C, utilize extraction by steam distillation, obtain oil-like extracts, accurately weigh
Weight is 0.074g；
(3) according to formula: oils and fats extracts yield=extract quality/sample mass * 100% and calculates this sample ether extraction
Oil yield is 10.45%；
(4) accurately weigh a small amount of extract, be configured to the solution that concentration is 0.8mg/mL, the filter membrane of mistake 0.45 μm to 2mL
Sample injection bottle, obtain GC-MS analyze need testing solution；
(5) utilizing gas chromatograph-mass spectrometer (GC-MS), be analyzed need testing solution, running parameter is as follows:
Gas phase condition: chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane (30m × 0.25mm × 0.25 μm)
Fused-silica capillary column；Heating schedule: column temperature 50 DEG C, is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, with 2 DEG C/min liter
Temperature, to 170 DEG C, keeps 10min, is warming up to 310 DEG C with 5 DEG C/min, keeps 5min；Temperature of vaporization chamber 250 DEG C；Carrier gas is high-purity
He (99.999%)；Carrier gas flux 1.0mL/min；Sample size 2.0 μ L, does not shunts, solvent delay time: 4.0min.
Mass Spectrometry Conditions: electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature
150℃；Interface temperature 280 DEG C；Scan pattern: full scan；Mass scan range m/z 55～500.
(6) analysis obtains chromatogram and mass spectrum, and mass spectrum is composed storehouse by Nist2014, Wiley275 and self-built Lignum Aquilariae Resinatum and entered
Row Qualitative Identification, and use areas of peak normalization method to calculate each component percentage contents, i.e. obtain this sample component and identify knot
Really, 3 it are shown in Table.
Table 3 GC-MS identifies the result of three components
This sample detects monomeric compound A:2-[2-(4-methoxyl group) phenethyl] chromone (38.03%), singulation
Compound B:2-(2-phenethyl) chromone (23.05%) and monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone
(6.38%).
(7) according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, testing sample is identified, specific as follows:
1. this sample ether extraction yield is 10.45%, more than 10%, meets identification of indicator setting；
2. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects [2-(the 4-methoxyl group of monomeric compound A:2-in this sample
Phenethyl)] relative amount of chromone is 38.03%, meet index regulation must not be less than 20%；
3. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects monomeric compound B:2-in this sample (2-phenethyl) color
The relative amount of ketone is 23.05%, and meet index regulation must not be less than 15%；
4. this sample is detected by gas chromatograph-mass spectrometer (GC-MS) (GC-MS), monomeric compound A:2-[2-(4-methoxyl group
Phenethyl)] relative amount of chromone is higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone.
5. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects monomeric compound C:6,7-dimethoxy-2-in this sample
The percentage contents of (2-phenethyl) chromone is 6.38%, and meet index regulation must not be higher than 10%.
(8) operations according to the instant invention code, this sample meets all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, and this sample is
Strange nanmu Lignum Aquilariae Resinatum.
(9) utilize identical analysis method to being to hang salty fragrant sample to identify through expert testimony, this sample description:
Outward appearance: spread pitchy oils and fats on yellow-white xylem, surface xylem becomes to hang thorn-like；Abnormal smells from the patient: have light fragrance；Feel:
Quality is light, and hands pinches surface without glutinous sense；State cut by cutter: be difficult to cutting, not rolling.Identify according to strange nanmu Lignum Aquilariae Resinatum identification of indicator,
Specific as follows:
1. this sample ether extraction yield is 0.45%, less than 10%, is unsatisfactory for strange nanmu Lignum Aquilariae Resinatum index setting；
2. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects [2-(the 4-methoxyl group of monomeric compound A:2-in this sample
Phenethyl)] relative amount of chromone is 0.00%, be unsatisfactory for index regulation must not be less than 20%；
3. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects monomeric compound B:2-in this sample (2-phenethyl) color
The relative amount of ketone is 5.68%, and be unsatisfactory for index regulation must not be less than 15%；
4. this sample is detected by gas chromatograph-mass spectrometer (GC-MS) (GC-MS), monomeric compound A:2-[2-(4-methoxyl group
Phenethyl)] relative amount of chromone less than the relative amount of monomeric compound B:2-(2-phenethyl) chromone, be unsatisfactory for strange nanmu mirror
Determine index；
5. gas chromatograph-mass spectrometer (GC-MS) (GC-MS) detects monomeric compound C:6,7-dimethoxy-2-in this sample
The percentage contents of (2-phenethyl) chromone is 15.89%, and be unsatisfactory for index regulation must not be higher than 10%.
(10) operations according to the instant invention code, this sample is unsatisfactory for all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, this sample
Product are strange nanmu Lignum Aquilariae Resinatum.
Embodiment 4:
Instrument: Agilent company 1260 of U.S. HPLC instrument, is equipped with automatic sampler, chem workstation；Beijing Sai Duolisi
Balance company limited BP221S ten thousand/electronic scale；Trade company of Lay Boke surname extraction instrument.
Reagent: Tianjin Chemical Reagents Factory No.1's ethanol (AR)；World company of the U.S. (Tedia) produces methanol (chromatographically pure)；Beautiful
World company of state (Tedia) produces acetonitrile (chromatographically pure)；Tianjin Chemical Reagents Factory No.1's formic acid (AR).
Consumptive material: 2mL sample injection bottle, 0.45 μm organic facies filter membrane.
Testing sample describes: it is blackish green that outward appearance is yellowish-brown colour band, strip and curly, the most deep mixed yellowish-brown
Oils and fats band is distributed on it, and oils and fats bar third dimension is obvious；On abnormal smells from the patient, aromatic flavor is mellow, sweet with as Olibanum taste and Mel
Taste；In feel, quality is thick and heavy, and hands pinches the glutinous sense in surface substantially；State cut by cutter: easily rolling.This sample is reflected by Senior Expert sense organ
Fixed, unanimously it is accredited as strange nanmu.
The authenticity of testing sample includes following step:
(1) pre-treatment of sample: take a fritter sample from this sample, shredding and accurately weighing weight is 1.380g；
(2) sample adds the alcohol solvent of 10mL, is heated to 110 DEG C, utilize surname extraction equipment to extract, obtain oily and carry
Take thing 0.358g；
(3) according to formula: oils and fats extracts yield=extract quality/sample mass * 100% and calculates this sample extraction oils and fats
Yield is 25.98%；
(4) accurately weigh a small amount of extract, be configured to the solution that concentration is 1mg/mL, cross organic microporous filter membrane of 0.45 μm
To the sample injection bottle of 2mL, obtain need testing solution；The most accurately weigh a small amount of monomeric compound A2-[2-(4-methoxybenzene second
Base)] chromone, monomeric compound B2-(2-phenethyl) chromone and monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) color
Ketone, is configured to the solution that concentration is 1mg/mL respectively, and the 0.45 organic microporous filter membrane of μm excessively, to the sample injection bottle of 2mL, obtains singulation
Compound solution A, monomeric compound B solution and monomeric compound C solution；
(5) utilize high performance liquid chromatograph, need testing solution and three monomeric compound solution are analyzed, work ginseng
Number is as follows:
Liquid-phase condition: Dionex-Acclaim 120 C18Chromatographic column (250mm × 4.6mm, 5 μm), flowing is acetonitrile mutually
(A) and 0.05% aqueous formic acid (B).Gradient program: 0～60min, 25%～55%A, 60～80min, 55%～
80%A, 80～90min, 80%～100%A, 90～95min, 100%A.Flow velocity 0.4mL min-1, detect wavelength 254nm, post
Temperature 30 DEG C, sample size 5 μ L.(6) obtain chromatogram, utilize the retention time of two monomeric compounds to this in testing sample two
Individual monomeric compound is identified, and uses areas of peak normalization method to calculate the relative of these three monomeric compound in testing sample
Percentage composition, qualification result is shown in Table 4.
Table 4 HPLC identifies the result of three components
| Numbering | Retention time | Compound name | Molecular formula | Molecular weight | Percentage contents |
| 1 | 64.05 | 6,7-dimethoxy-2-(2-phenethyl) chromone | C19H18O4 | 310 | 0.25% |
| 2 | 69.50 | 2-[2-(4-methoxyl group) phenethyl] chromone | C18H16O3 | 280 | 24.47% |
| 3 | 71.43 | 2-(2-phenethyl) chromone | C17H14O2 | 250 | 17.32% |
This sample detects monomeric compound A:2-[2-(4-methoxyl group) phenethyl] chromone (24.47%), singulation
Compound B:2-(2-phenethyl) chromone (17.32%) and monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone
(0.25%).
(7) according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, testing sample is identified, specific as follows:
1. this sample extraction oil yield is 25.98%, and more than 10%, touch the mark setting；
2. high performance liquid chromatograph (HPLC) detects [2-(the 4-methoxybenzene second of monomeric compound A:2-in this sample
Base)] relative amount of chromone is 24.47%, meet index regulation must not be less than 20%；
3. high performance liquid chromatograph (HPLC) detects the phase of monomeric compound B:2-in this sample (2-phenethyl) chromone
Being 17.32% to content, meet index regulation must not be less than 15%；
4. this sample is detected by high performance liquid chromatograph (HPLC), monomeric compound A:2-[2-(4-methoxybenzene second
Base)] relative amount of chromone is higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone.
5. high performance liquid chromatograph (HPLC) detects monomeric compound C:6,7-dimethoxy-2-(2-benzene in this sample
Ethyl) percentage contents of chromone is 0.25%, meet index regulation must not be higher than 10%.
(8) operations according to the instant invention code, this sample meets all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, and this sample is
Strange nanmu Lignum Aquilariae Resinatum.
(9) utilize identical analysis method that the sample being artificial agilawood through expert testimony is identified, this sample description:
Outward appearance: spreading pitchy oils and fats in white wooden portion, there is baked wheaten cake vestige sample side；Abnormal smells from the patient: distribute simple and elegant fragrance；Feel:
Quality is light, and hands pinches surface without glutinous sense；State cut by cutter: easily cut, not rolling.Identify according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, tool
Body is as follows:
1. this sample extraction oil yield is 5.51%, and less than 10%, fall short of the target setting；
2. high performance liquid chromatograph (HPLC) detects [2-(the 4-methoxybenzene second of monomeric compound A:2-in this sample
Base)] relative amount of chromone is 5.35%, be unsatisfactory for index regulation must not be less than 20%；
3. high performance liquid chromatograph (HPLC) detects the phase of monomeric compound B:2-in this sample (2-phenethyl) chromone
Being 0.00% to content, be unsatisfactory for index regulation must not be less than 15%；
4. this sample is detected by high performance liquid chromatograph (HPLC), monomeric compound A:2-[2-(4-methoxybenzene second
Base)] relative amount of chromone higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone, meet strange nanmu and identify and refer to
Mark；
5. high performance liquid chromatograph (HPLC) detects monomeric compound C:6,7-dimethoxy-2-(2-benzene in this sample
Ethyl) percentage contents of chromone is 7.65%, meet index regulation must not be higher than 10%.
(10) operations according to the instant invention code, the most 3. this sample is unsatisfactory for the index of strange nanmu Lignum Aquilariae Resinatum authenticity, should
Sample is not strange nanmu Lignum Aquilariae Resinatum.
Embodiment 5:
Instrument: Micromass company of Britain GCT type gas chromatogram-flight time mass spectrum；Beijing Sai Duolisi balance is limited
Company's BP221S ten thousand/electronic scale；U.S.'s Bransonic-5510E-DTH ultrasonic washing instrument；SITEC company of Switzerland surpasses
Supercritical fluid extraction instrument HP-SFE.
Reagent: industrial liquid CO2(purity > 99.0%, the pungent gas companies in Ningbo side)；World company of the U.S. (Tedia) produces
Methanol (chromatographically pure).
Consumptive material: 2mL sample injection bottle, 0.45 μm organic facies microporous filter membrane.
Testing sample describes: block wood particle in appearance, and surface is puce, and seen from have brown oils and fats stria to divide
Cloth；Sweet taste and milk aromatic flavor on abnormal smells from the patient；In feel, quality is general, and hands pinches surface glutinous sense；State cut by cutter: can slightly rolling.Should
Sample is identified by Senior Expert sense organ, is unanimously accredited as strange nanmu.
The authenticity of testing sample includes following step:
(1) pre-treatment of sample: take a fritter sample from this, shredding and accurately weighing weight is 0.405g, with 2.00g
Kieselguhr mix homogeneously, obtains sample to be analyzed；
(2) above-mentioned band being analyzed sample and load extraction pond, void volume kieselguhr fills up.Pond and supercritical fluid will be extracted
Extraction equipment connects, and extracts.Extraction conditions is: static extracting time 10min, dynamic extraction time 60min, pressure
20MPa, temperature 50～70 DEG C, CO2Flow velocity 2L/min；Entrainer flow 0.4mL/min.Extract receiving flask is collected.Accurately
Weighing weight is 0.1108g；
(3) according to formula: oils and fats extracts yield=extract quality/sample mass * 100% and calculates this sample ether extraction
Oil yield is 27.38%；
(4) accurately weigh a small amount of extract, be configured to the solution that concentration is 0.8mg/mL, the filter membrane of mistake 0.45 μm to 2mL
Sample injection bottle, obtain need testing solution；
(5) utilizing GC-TOFMS instrument, be analyzed need testing solution, running parameter is as follows:
Gas phase condition: chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane (30m × 0.25mm × 0.25 μm)
Fused-silica capillary column；Heating schedule: column temperature 50 DEG C, is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, with 2 DEG C/min liter
Temperature, to 170 DEG C, keeps 10min, is warming up to 310 DEG C with 5 DEG C/min, keeps 5min；Temperature of vaporization chamber 250 DEG C；Carrier gas is high-purity
He (99.999%)；Carrier gas flux 1.0mL/min；Sample size 1.0 μ L, split ratio: 10:1, solvent delay time: 4.0min.
Mass Spectrometry Conditions: electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature
150℃；Interface temperature 280 DEG C；Scan pattern: full scan；Resolution: 8000FWHM.
(6) analysis obtains chromatogram and mass spectrum, and mass spectrum is composed storehouse by Nist2014, Wiley275 and self-built Lignum Aquilariae Resinatum and entered
Row Qualitative Identification, and use areas of peak normalization method to calculate each component percentage contents, i.e. obtain this sample component and identify knot
Really, 5 it are shown in Table.
Table 5 GC-TOFMS identifies the result of three components
This sample detects monomeric compound A:2-[2-(4-methoxyl group) phenethyl] chromone (27.92%) and singulation
Compound B:2-(2-phenethyl) chromone (19.98%), is not detected by monomeric compound C:6,7-dimethoxy-2-(2-benzene second
Base) chromone.
(7) according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, testing sample is identified, specific as follows:
1. this sample extraction oil yield is 27.38%, and more than 10%, touch the mark setting；
2. gas chromatogram-time of-flight mass spectrometer (GC-TOFMS) detects monomeric compound A:2-[2-(4-in this sample
Methoxyphenethyl)] relative amount of chromone is 27.92%, meet index regulation must not be less than 20%；
3. gas chromatogram-time of-flight mass spectrometer (GC-TOFMS) detects monomeric compound B:2-(2-benzene in this sample
Ethyl) relative amount of chromone is 19.98%, meet index regulation must not be less than 15%；
4. this sample is detected by gas chromatogram-time of-flight mass spectrometer (GC-TOFMS), monomeric compound A:2-[2-
(4-methoxyphenethyl)] relative amount of chromone is higher than the relative amount of monomeric compound B:2-(2-phenethyl) chromone.
5. this sample is not detected by monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone, meets and refer to
What mark specified must not be higher than 10%.
(8) operations according to the instant invention code, this sample meets all indexs of strange nanmu Lignum Aquilariae Resinatum authenticity, and this sample is
Strange nanmu Lignum Aquilariae Resinatum.
(9) identical analysis method is utilized to identify for the sample of haze wax Lignum Aquilariae Resinatum through expert testimony, this sample description:
Outward appearance: gather on the yellow-white xylem of surface yellowish-brown oils and fats, and there is bark sample side；Abnormal smells from the patient: emanating faint scent；Feel:
Quality is light, and hands pinches surface without glutinous sense；State cut by cutter: easily cut, not rolling.Identify according to strange nanmu Lignum Aquilariae Resinatum identification of indicator, tool
Body is as follows:
1. this sample extraction oil yield is 7.42%, and less than 10%, fall short of the target setting；
2. gas chromatogram-time of-flight mass spectrometer (GC-TOFMS) detects monomeric compound A:2-[2-(4-in this sample
Methoxyphenethyl)] relative amount of chromone is 5.24%, be unsatisfactory for index regulation must not be less than 20%；
3. gas chromatogram-time of-flight mass spectrometer (GC-TOFMS) detects monomeric compound B:2-(2-benzene in this sample
Ethyl) relative amount of chromone is 21.05%, meet index regulation must not be less than 15%；
4. this sample is detected by gas chromatogram-time of-flight mass spectrometer (GC-TOFMS), monomeric compound A:2-[2-
(4-methoxyphenethyl)] relative amount of chromone is less than the relative amount of monomeric compound B:2-(2-phenethyl) chromone, no
Meet strange nanmu identification of indicator；
5. relative amount monomeric compound C:6,7-dimethoxy-2-(2-phenethyl) chromone being detected in this sample is
9.47%, meet index regulation must not be higher than 10%.
(10) operations according to the instant invention code, the most 4. this sample is unsatisfactory for the index of strange nanmu Lignum Aquilariae Resinatum authenticity, should
Sample is not strange nanmu Lignum Aquilariae Resinatum.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. the method identifying the strange nanmu Lignum Aquilariae Resinatum true and false, it is characterised in that including:
Step 1, testing sample is extracted, it is thus achieved that extract, calculate grease extraction efficiency simultaneously；
Step 2, extract obtain monomeric compound 2-[2-(4-methoxybenzene second in testing sample by chemical analysis method
Base)] percentage contents of chromone, the percentage contents of monomeric compound 2-(2-phenethyl) chromone and monomeric compound 6,
The percentage contents of 7-dimethoxy-2-(2-phenethyl) chromone；
Step 3, testing sample are accredited as strange nanmu Lignum Aquilariae Resinatum simultaneously when meeting following standard；
(1) testing sample oils and fats extracts yield and must not be less than 10%；
(2) in testing sample, the percentage contents of monomeric compound 2-[2-(4-methoxyphenethyl)] chromone must not be less than
20%；
(3) in testing sample, the percentage contents of monomeric compound 2-(2-phenethyl) chromone must not be less than 15%；
(4) in same testing sample, the percentage contents of 2-[2-(4-methoxyphenethyl)] chromone is higher than 2-(2-phenethyl)
The percentage contents of chromone；
(5) in testing sample, the percentage contents of monomeric compound 6,7-dimethoxy-2-(2-phenethyl) chromone must not be big
In 10%.
Method the most according to claim 1, it is characterised in that described in be extracted as organic solvent extraction, surname extraction, titanium dioxide
Carbon supercritical extraction or vapor distillation extract.
Method the most according to claim 2, it is characterised in that described organic solvent includes ethyl acetate, ether, ethanol, just
Hexane, petroleum ether, chloroform, methanol, n-butyl alcohol, alkane, benzene, acetone.
Method the most according to claim 1, it is characterised in that described chemical analysis method includes: gas chromatogram, gas phase color
Spectrum-mass spectrometry, gas chromatogram-flight time mass spectrum, fast pyrogenation-gas chromatography mass spectrometry, (ultra high efficiency/efficient) liquid chromatograph, height
Speed adverse current chromatogram, (ultra high efficiency/efficient) liquid chromatograph mass spectrography, efficient liquid phase-flight time mass spectrum, shooting flow body colour
Spectrum-mass spectrometry.
Method the most according to claim 4, it is characterised in that described gas chromatogram, gas chromatography-mass spectrography, gas phase color
In spectrum-flight time mass spectrum condition, gas phase condition is as follows:
Chromatographic column: HP-5MS 5%Phenyl Methyl Siloxane fused-silica capillary column；Heating schedule: column temperature 50
DEG C, it is warming up to 150 DEG C with 5 DEG C/min, keeps 20min, be warming up to 170 DEG C with 2 DEG C/min, keep 10min, with 5 DEG C/min liter
Temperature, to 310 DEG C, keeps 5min；Temperature of vaporization chamber 250 DEG C.
Method the most according to claim 4, it is characterised in that when described gas chromatography-mass spectrography, gas chromatogram-flight
Between in mass spectrum, (ultra high efficiency/efficiently) liquid chromatograph mass spectrography Mass Spectrometry Conditions one of following:
(1) electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature 150 DEG C；Interface temperature
Spend 280 DEG C；Scan pattern: full scan；Mass scan range m/z 55～500；
(2) electron bombardment (EI) ion source；Electron energy 70eV；Ion source temperature 230 DEG C；Quadrupole rod temperature 150 DEG C；Interface temperature
Spend 280 DEG C；Scan pattern: full scan；Resolution: 8000FWHM；
(3) ESI ion source；Collision gas is helium, 0.4L/min；Atomization drying gas is high pure nitrogen (99.999%),
6.0L/min；Capillary voltage-4000V；End plate voltage 500V；Nebulizer pressure 15psi；Mass scan range m/z 70to
2200。
Method the most according to claim 4, it is characterised in that described (ultra high efficiency/efficient) liquid chromatograph, (ultra high efficiency/height
Effect) liquid-phase condition is as follows in liquid chromatograph mass spectrography:
Dionex-Acclaim 120 C18Chromatographic column, mobile phase A is acetonitrile, and Mobile phase B is 0.5% aqueous formic acid, eluting ladder
Degree program: 0～60min, 25%～55%A, 60～80min, 55%～80%A, 80～90min, 80%～100%A, 90～
95min, 100%A；Flow velocity 0.4mL min-1, detect wavelength 254nm.
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| 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 |
| CN111272899A (en) * | 2020-03-11 | 2020-06-12 | 中国热带农业科学院热带生物技术研究所 | Method for identifying agilawood produced by thermal department No. 2 |
| CN112773004A (en) * | 2020-12-29 | 2021-05-11 | 海南贵本南药科技有限公司 | Heating non-combustible Qinan agilawood cigarette product |
| CN112772962A (en) * | 2020-12-31 | 2021-05-11 | 海南黎药堂生物科技开发有限公司 | Tobacco shred and cigarette containing aquilaria sinensis extract and preparation method of tobacco shred and cigarette |
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