CN105136960A - Method for detecting and distinguishing odor components of donkey hide, horse hide or cattle hide as well as distinguishing standard thereof - Google Patents
Method for detecting and distinguishing odor components of donkey hide, horse hide or cattle hide as well as distinguishing standard thereof Download PDFInfo
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Abstract
The invention discloses a method for detecting and distinguishing odor components of a donkey hide, a horse hide or a cattle hide as well as a distinguishing standard thereof. The odor components of the donkey hide, the horse hide and the cattle hide are extracted by adopting head space solid phase microextraction; the composition is detected by adopting a gas chromatography-mass spectrometry method, a material basis forming the odor is researched, main difference components are found out, peculiar odor components of various hides are determined, the peculiar odor components are taken as a standard, the detected odor components of a sample to be detected are looked up from the obtained standard to determine the source of the sample to be detected, preliminary data and theory basises are provided for the quality control of the donkey hide, and the problem of how to well control the quality of the donkey hide in the production of donkey-hide gelatin, for ensuring the accuracy and reliability of sources of raw materials in the donkey-hide gelatin production is solved.
Description
Technical field
The present invention relates to and a kind ofly detect and differentiate donkey, the method for horse or ox-hide odour component and judging standard thereof, be specially the method being differentiated donkey, horse and ox-hide by headspace solid-phase microextraction-gas chromatography/mass spectrometry technology by analysis of volatile components, the invention belongs to technical field of analysis and detection.
Background technology
Version " Chinese Pharmacopoeia " regulation in 2010
[1], donkey-hide gelatin be the dry skin of equine species donkey EquusasinusL. or fresh hide through decocting, the concentrated solid gum made.And the quality standard of donkey hide is not included in " Chinese Pharmacopoeia " always.Due to the driving of economic interests, market occur often with ox-hide, horse skin and mix the shoddy donkey-hide gelatin that skin makes, while infringement consumer's interests, bringing a new difficult problem also to the quality control of donkey-hide gelatin.This problem is in the production of enterprise, and the most frequently used donkey hide discrimination method is that proterties is differentiated.And for the onal of drying, the difficulty of discriminating strengthens, even the technician known a thing or two also is difficult to distinguish the hide of donkey and ox, horse.And donkey is different with the physiological make-up of the health of ox, horse, the environment of life is also variant, and thus the difference of its body odour is larger.There is not been reported in the current research about the smell identification of donkey hide.
Solid-phase microextraction (solid-phasemicroextraction, SPME) technology belongs to non-solvent selective extraction method, there is centralized procurement sample, absorption, extraction, concentrated, sample introduction in one, can with GC, GC/MS, HPLC, HPLC/MS coupling, exempt from solvent, outstanding advantage quick, simple to operate and be widely used in the mensuration of the volatile ingredients such as environment, food, aquatic products, Chinese medicine
[2-6].
Summary of the invention:
The present invention aims to provide a kind of method, judging standard and the method that detect donkey horse ox-hide odour component, adopt headspace solid-phase microextraction technology to extract donkey, the odour component of horse and ox-hide is volatile ingredient, the method of gas chromatography-mass spectrography is adopted to detect its composition, inquire into the material base that its smell is formed, find out its Main Differences component, quality control for donkey hide provides preliminary data and rationale, solve during donkey-hide gelatin is produced and how to control the quality of donkey hide well, ensure the accuracy of raw material sources that donkey-hide gelatin is produced and the problem of reliability.
For achieving the above object, technical scheme of the present invention is:
Detect a method for donkey, horse or ox-hide odour component, the method is that this technical step is by headspace solid-phase microextraction-gas chromatography/mass spectrometry technology:
1) pretreatment of raw material;
2) headspace solid-phase microextraction: added by sample in ml headspace bottle, inserts fiber head, and adjustment is the position of fixed extractor head in head space volume also, extracts;
3) gas chromatography/mass spectrometry detects: regulate chromatographic condition and Mass Spectrometry Conditions, to step 2) in extraction volatile constituent carry out detections also Analysis and Identification.
The present invention also has following additional technical feature:
Preferably, described pretreatment of raw material is cut off by the hair on the hide of donkey, horse or ox respectively, clean with water rinse, then uses deionized water rinsing, and put and dry to constant weight in 40 DEG C of baking ovens, be cut into small pieces, comminutor is pulverized, and crosses 100 mesh sieves.
Preferably, described headspace solid-phase microextraction method is: extracting fiber head is at injection port 240 DEG C of aging 30min of gas chromatography, do blank for several times again under the chromatographic condition identical with detecting sample, until the chromatographic peak of resolving blank extracting head does not change, add the 1g hide sample accurately taken in 10mL ml headspace bottle, at 50 DEG C, balance 30min, insert 65 μm of PDMS/DVB fiber heads, adjustment is the position of fixed extractor head in head space volume also, in 50 DEG C of extraction 30min.
Preferably, described chromatographic condition is: chromatographic column: Agilent19091J-433-HP-5 capillary column (30m × 250 μm × 0.25 μm); Heating schedule: 60 DEG C keep 2min, and 5 DEG C/min rises to 230 DEG C, keep 20min; Carrier gas (He) flow velocity 1.0mL/min, injector temperature: 250 DEG C; Input mode: Splitless injecting samples; Desorption time: 5min.
Preferably, described Mass Spectrometry Conditions is: electronics bombardment (EI) ion gun; Electron energy 70eV; Transmission line temperature 230 DEG C; Ion source temperature 170 DEG C; Ion hydrazine temperature 150 DEG C, mass scan range m/z30 ~ 800.
Preferably, above-mentioned steps 3) described in Analysis and Identification method be: to peak each in total ion current figure after scanning of the mass spectrum, obtain full scan mass spectrogram, resolve collection of illustrative plates and obtain related data, by comparing with mass spectrometric data system NIST and Willey standard diagram database, qualitative, quantitative being carried out to volatile constituent, determining the volatile constituent in donkey hide, horse skin or ox-hide and content.
Preferably, the normalized method of integral area is adopted to determine the percentage contents of each component in volatile constituent.
Present invention also offers a kind of standard utilizing odour component discriminating donkey hide, this standard is used for the match parameters of volatile constituent and its standard that will obtain, and this standard comprises following parameter:
The peculiar volatile constituent of donkey hide comprises 16 kinds, it is 36.26% that described peculiar volatile constituent percentage contents in volatile constituent accounts for, and each component and percentage contents thereof are respectively: n-hexyl aldehyde 1.92%, enanthaldehyde 2.40%, 1-(2-hydroxy-4-methoxyphenyl) ethyl ketone 2.58%, acetic acid 5.33%, propionic acid 2.63%, butyric acid 5.23%, 2-Methyl Butyric Acid 2.61%, 3 Methylbutanoic acid 4.05%, 2-(2-Butoxyethoxy) acetate ethanol ester 0.95%; Chain hydrocarbon: 2-methyl isophthalic acid-trifluoroacetyl group pentane 0.51%, 1,1'-2-propyl group-1,3-propylidene) bicyclohexane 1.20%, eicosane 1.32%, (E)-9-eicosylene 1.28%, aromatic hydrocarbon, comprises phenol 2.4%, biphenyl 0.85%; A small amount of alcohol: (E)-2-decen-1-ol 0.99%.
Preferably, also comprise the standard differentiating horse or ox-hide, its parameter is as follows respectively:
1) the peculiar volatile constituent of horse skin comprises 14 kinds, described peculiar volatile constituent percentage contents in volatile constituent is 16.31%, each component and percentage contents thereof are respectively: 14-vaccenic acid aldehyde 3.83%, 6,10-dimethyl-2-undecyl ketone 0.45%, 2-HEPTANONE 1.49%, 5-heptyl dihydro-2 (3 hydrogen)-furanone 0.72%, 2-1-methyl ethylidene cyclohexanone 1.15%, oxalic acid decyl propyl diester 2.02%, sulphurous acid hexyl octyl group ester 0.36%; Nitrogen-containing compound: 2-ethyl acridine 0.09%, 3-crotonamide 0.71%, 4-methyl-2 pentanone dimethyl hydrazone 0.12%, propionamide 0.04%, cis-3,4-dimethyl-2-phenyl tetrahydrochysene-Isosorbide-5-Nitrae-thiazine 1.75%; Unsaturated hydrocarbon: E-3-nonene 2.1%, 4-nonene 1.48%;
2) the peculiar volatile constituent of ox-hide comprises 8 kinds, described peculiar volatile constituent percentage contents in volatile constituent is 17.57%, and each component and percentage contents thereof are respectively: 6-methyl-Benzaldehyde,2-hydroxy 1.92%, 6-methyl-2-HEPTANONE 1.44%, (Z)-14-tricosenoic acid 4.06%, ethyl caprilate 3.52%, ethyl pelargonate 1.44%; The chloro-4-of 2-(4-methoxyphenyl)-6-(4-nitrobenzophenone) pyrimidine 1.47%; Aromatic hydrocarbon: benzepine 2.18%; Alcohol: 2-methyl-1-butene alcohol 1.54%.
The present invention also provides a kind of method utilizing odour component to differentiate donkey, horse or ox-hide, and the method step is:
1) testing sample is determined its volatile constituent according to the method for above-mentioned detection donkey, horse or ox-hide odour component;
2) by step 1) in the volatile constituent determined search in the parameter described in above-mentioned standard, the peculiar volatile ingredient determination testing sample according to finding is donkey hide, or
By step 1) in the volatile constituent determined carry out searching coupling in above-mentioned parameter, the result determination testing sample according to coupling is corresponding donkey, horse or ox-hide.
Advantage of the present invention is:
Present invention employs headspace solid-phase microextraction-gas chromatography/mass spectrometry technology by odour component analysis and identification donkey, the method of horse and ox-hide, by detecting donkey respectively, the volatile ingredient of horse and ox-hide and content thereof determine each seed coat endemic element and as standard, the source that institute's test sample product are corresponding can be determined compared with the component contained in detected sample according to the endemic element of often kind of source hide in standard, testing process exempts from solvent, fast, simple to operate, result is accurate, method is easy, the detection of donkey-hide gelatin raw material in donkey-hide gelatin commercial production can be widely used in, determine raw material sources.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing illustrates:
Fig. 1 is each constituents and the relative content graph of a relation thereof of donkey hide, horse skin and ox-hide volatile ingredient;
Fig. 2 is each constituents and the kind number graph of a relation thereof of donkey hide, horse skin and ox-hide volatile ingredient.
Embodiment
Below in conjunction with instantiation, the present invention is described in detail.
Embodiment 1
1 materials and methods
1.1 materials and instrument
Donkey hide, horse skin, ox-hide sample are provided by Donga donkey-hide gelatin incorporated company; Manual solid-phase micro-extraction (SPME) device, 65 μm of dimethyl silicone polymer one divinyl benzene copolymer (PDMS/DVB) extracting fiber heads, Supelco company; Agilent7890A/5973N gas chromatograph-mass spectrometer, Agilent19091J-433-HP-5 capillary column (30m × 250 μm × 0.25 μm), Agilent company of the U.S.; BS110S electronic balance, Beijing Sai Duolisi balance company limited; SF-130 type high speed medicinal herb grinder, Zhongnan (South Contral) Pharmacentical Machinery Fectory.
1.2 method
1.2.1 Feedstock treating
Respectively the hair on the hide of donkey, horse, ox is cut off, clean with tap water rinse, then use deionized water rinsing three times, put and dry to constant weight in 40 DEG C of baking ovens, be cut into the fritter of about 1cm × 1cm, Universalpulverizer is pulverized, and crosses 100 mesh sieves.
1.2.2 headspace solid-phase microextraction
Extracting fiber head at injection port 240 DEG C of aging 30min of gas chromatography, then does blank for several times, until the chromatographic peak of resolving blank extracting head does not change under the chromatographic condition identical with detecting sample.Add the 1g hide sample accurately taken in 10mL ml headspace bottle, balance 30min at 50 DEG C, insert 65 μm of PDMS/DVB fiber heads, adjustment is the position of fixed extractor head in head space volume also, in 50 DEG C of extraction 30min.
1.2.3 chromatographic condition
Chromatographic column: Agilent19091J-433-HP-5 capillary column (30m × 250 μm × 0.25 μm); Heating schedule: 60 DEG C keep 2min, and 5 DEG C/min rises to 230 DEG C, keep 20min; Carrier gas (He) flow velocity 1.0mL/min, injector temperature: 250 DEG C; Input mode: Splitless injecting samples.Desorption time: 5min.
1.2.4 Mass Spectrometry Conditions
Electronics bombardment (EI) ion gun; Electron energy 70eV; Transmission line temperature 230 DEG C; Ion source temperature 170 DEG C; Ion hydrazine temperature 150 DEG C, mass scan range m/z30 ~ 800.
2 results and discussion
To peak each in total ion current figure after scanning of the mass spectrum, retrieved by mass spectrometric data system (NIST and Willey standard diagram database), and combine artificial parsing, identify the volatile ingredient in donkey hide, horse skin and ox-hide, adopt the normalized method of integral area to determine the percentage contents of each component in volatile constituent, the component of mass number more than 80 (full marks are 100) is just reported.Analysis result is in table 1.
Table 1GC-MS analyzes the volatile ingredient of donkey hide, horse skin and ox-hide
2.1 volatile ingredient compositions
From donkey hide, horse skin and ox-hide, identify 50 kinds of volatile ingredients altogether, mainly comprise ketone compounds, aldehyde compound, carboxylic acids, nitrogen-containing compound, chain hydrocarbon (alkane and alkene), aromatic hydrocarbon, ester class and alcohol compound.The kind of volatile constituent identified in three kinds of hides and the relation of quantity are shown in Fig. 1, Fig. 2.
27 kinds of odour components are identified altogether, comprising 3 kinds of ketone, 5 kinds of aldehyde, 7 kinds of chain hydrocarbons, 5 kinds of acid, 4 kinds of aromatic hydrocarbon, a kind of nitrogen-containing compound, a kind of ester and a kind of alcohol from donkey hide.Wherein chain hydrocarbon accounts for 33.51% of whole component concentration, and aldehydes accounts for 22.14%, and acids accounts for 19.85%, and ketone accounts for 13.87%, and aromatic hydrocarbon accounts for 7.60%, and nitrogen-containing compound accounts for 1.09%, and ester class accounts for 0.95%.The compound that content is larger is n-tridecane (17.57%), n-dodecane (7.48%), aldehyde C-9 (6.81%), benzaldehyde (7.53%), 2-decanone (9.11%), acetic acid (5.33%), butyric acid (5.23%), 3 Methylbutanoic acid (4.05%), n-tetradecane (4.14%), octanal (3.48%), accounts for 70.73% of total component concentration.
22 kinds of odour components are identified altogether, comprising 7 kinds of ketones, 3 kinds of aldehydes, 6 kinds of nitrogen-containing compounds, 3 kinds of chain hydrocarbons, 2 kinds of esters and a kind of aromatic hydrocarbon from horse skin.Wherein ketone compounds accounts for 77.06% of whole component concentration, and aldehydes accounts for 10.17%, and chain hydrocarbon accounts for 6.64%, and nitrogen-containing compound accounts for 3.08%, and ester class accounts for 2.38%, and aromatic hydrocarbon accounts for 0.68%.The compound that wherein content is larger is 2-decanone (41.20%), methyl n-heptyl ketone (26.82%), methyln-hexyl ketone (5.23%), aldehyde C-9 (4.57%), accounts for 77.82% of total component concentration.
17 kinds of odour components are identified altogether, comprising 4 kinds of ketones, 3 kinds of aldehydes, 3 kinds of chain hydrocarbons, 3 kinds of aromatic hydrocarbon, 2 kinds of esters, a kind of acid and a kind of alcohol from ox-hide.Wherein ketone compounds accounts for 64.21% of whole component concentration, and aldehydes accounts for 5.79%, and alkane accounts for 15.45%, and aromatic hydrocarbon accounts for 3.97%, and ester class accounts for 4,96%, and alcohols accounts for 1.54%.The compound that content is larger is 2-decanone (35.21%), methyl n-heptyl ketone (23.34%), n-tridecane (8.57%), methyln-hexyl ketone (4.22%), methyln-hexyl ketone (4.22%), aldehyde C-9 (4.57%), (Z)-14-tricosenoic acid (4.06%), accounts for 75.4% of total component concentration.
2.2 3 kinds of hides have volatile constituent
The volatile constituent that donkey hide, horse skin and ox-hide have has aldehyde C-9,2-decanone, methyln-hexyl ketone, n-tridecane, but content difference is larger.The content of aldehyde C-9 in donkey, horse, ox-hide is 6.81%, 4.57%, 1.93% respectively; The content of methyln-hexyl ketone is 2.18%, 5.23%, 4.22% respectively; The content of n-tridecane is 17.57%, 3.06%, 8.57% respectively.
Donkey hide and horse skin have 3 kinds of total volatile constituents: benzaldehyde (content is respectively 7.53%, 1.77%), 2,6-dimethyl pyrazines (content is respectively 1.09%, 0.36%), 1-methylnaphthalene (content is respectively 1.26%, 0.68%); Horse skin and ox-hide only have a kind of total volatile constituent: methyl n-heptyl ketone (content is respectively 26.82%, 23.34%); Donkey hide and ox-hide have 3 kinds of total volatile constituents: octanal (content is respectively 3.48%, 1.94%), n-dodecane (content is respectively 7.48%, 3.97%), n-tetradecane (content is respectively 4.14%, 2.91%).
The peculiar volatile constituent of 2.3 3 kinds of hides
The peculiar volatile constituent of donkey hide has 16 kinds, content accounts for 36.26% of total component, mainly carbonyls: n-hexyl aldehyde (1.92%), enanthaldehyde (2.40%), 1-(2-hydroxy-4-methoxyphenyl) ethyl ketone (2.58%), acetic acid (5.33%), propionic acid (2.63%), butyric acid (5.23%), 2-Methyl Butyric Acid (2.61%), 3 Methylbutanoic acid (4.05%), 2-(2-Butoxyethoxy) acetate ethanol ester (0.95%); Chain hydrocarbon: 2-methyl isophthalic acid-trifluoroacetyl group pentane (0.51%), 1,1'-(2-propyl group-1,3-propylidene) bicyclohexane (1.20%), eicosane (1.32%), (E)-9-eicosylene (1.28%), aromatic hydrocarbon, comprises phenol (2.4%), biphenyl (0.85%); A small amount of alcohol: (E)-2-decen-1-ol (0.99%).
The peculiar volatile constituent of horse skin has 14 kinds, content accounts for 16.31% of total component, mainly carbonyls: 14-vaccenic acid aldehyde (3.83%), 6,10-dimethyl-2-undecyl ketones (0.45%), 2-HEPTANONE (1.49%), 5-heptyl dihydro-2 (3 hydrogen)-furanone (0.72%), 2-(1-methyl ethylidene) cyclohexanone (1.15%), oxalic acid decyl propyl diester (2.02%), sulphurous acid hexyl octyl group ester (0.36%); Nitrogen-containing compound: 2-ethyl acridine (0.09%), 3-crotonamide (0.71%), 4-methyl-2 pentanone dimethyl hydrazone (0.12%), propionamide (0.04%), cis-3,4-dimethyl-2-phenyl tetrahydrochysene-Isosorbide-5-Nitrae-thiazine (1.75%); Unsaturated hydrocarbon: (E)-3-nonene (2.1%), 4-nonene (1.48%).
The peculiar volatile constituent of ox-hide comprises 8 kinds, described peculiar volatile constituent percentage contents in volatile constituent is 17.57%, and each component and percentage contents thereof are respectively: 6-methyl-Benzaldehyde,2-hydroxy 1.92%, 6-methyl-2-HEPTANONE 1.44%, (Z)-14-tricosenoic acid 4.06%, ethyl caprilate 3.52%, ethyl pelargonate 1.44%; The chloro-4-of a small amount of nitrogen-containing compound: 2-(4-methoxyphenyl)-6-(4-nitrobenzophenone) pyrimidine 1.47%; Aromatic hydrocarbon: benzepine 2.18%; Alcohol: 2-methyl-1-butene alcohol 1.54%.
3 conclusions
3.1 solid-phase microextractions are applicable to the odour component detection of donkey, horse, ox-hide, the odour component of three kinds of hides can be distinguished, detect 50 kinds of volatile ingredients altogether, detect 27 kinds, 22 kinds and 17 kinds of odour components in donkey, horse, ox-hide respectively.
3.2 researchs detect four kinds of total volatile constituents of three kinds of hides altogether, are aldehyde C-9 respectively, 2-decanone, methyln-hexyl ketone, n-tridecane, but content difference is larger.Donkey hide and ox-hide have 3 kinds of total volatile constituents, and horse skin and ox-hide only have a kind of total volatile constituent, and donkey hide and horse skin have 3 kinds of total volatile constituents.
3.3 detect 16,14 and 8 kind of peculiar volatile ingredient respectively in donkey, horse, ox-hide, content account for respectively donkey, horse, ox-hide volatile ingredient total amount 36.26%, 17.57% and 16.31%, can as differentiate donkey, horse, ox-hide reference frame.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.
List of references
[1] Chinese Pharmacopoeia Commission. Pharmacopoeia of People's Republic of China [M]. one. Beijing: Chemical Industry Press, 2010:175.
[2] Feng Lin. volatile fatty acid in Headspace SPME-GC wastewater measurement. physical and chemical inspection-chemical fascicle [J] .2011,47 (1): 86 ~ 89.
[3] Ma Yulu, Zhu Bin, Zhang Lei, Xu Xinrong. headspace solid-phase microextraction-gas chromatography mass spectrometry detects pork freshness. Food Science [J] .2011,32 (14): 253 ~ 256.
[4] Tao Chen, kingly way is put down, Yang your pupil, Luo Yanan. and solid-phase microextraction GC-MS is to the mensuration of 8 kinds of apple fragrance components. Gansu Agriculture University's journal [J] .2011,46 (1): 122 ~ 126.
[5] Wei Yongsheng, Yang Zhen, Zheng Minyan, Geng Wei. SPME-GC/MS analyzes Ledum palustre volatile ingredient. Guangdong chemical industry [J] .2011,38 (3): 120 ~ 122.
[6] Wang Lu, Wang Xichang, Liu Yuan. grass carp different parts smell is studied. Food Science [J] .2010,31 (6): 158 ~ 164.
Claims (10)
1. detect a method for donkey, horse or ox-hide odour component, it is characterized in that, the method is that this technical step is by headspace solid-phase microextraction-gas chromatography/mass spectrometry technology:
Pretreatment of raw material;
Headspace solid-phase microextraction: added by sample in ml headspace bottle, inserts fiber head, and adjustment is the position of fixed extractor head in head space volume also, extracts;
Gas chromatography/mass spectrometry detects: regulate chromatographic condition and Mass Spectrometry Conditions, to step 2) in extraction volatile constituent carry out detections also Analysis and Identification.
2. method according to claim 1, is characterized in that, described pretreatment of raw material is cut off by the hair on the hide of donkey, horse or ox respectively, clean with water rinse, then use deionized water rinsing, put and dry to constant weight in 40 DEG C of baking ovens, be cut into small pieces, comminutor is pulverized, and crosses 100 mesh sieves.
3. method according to claim 1, it is characterized in that, described headspace solid-phase microextraction method is: extracting fiber head is at injection port 240 DEG C of aging 30min of gas chromatography, do blank for several times again under the chromatographic condition identical with detecting sample, until the chromatographic peak of resolving blank extracting head does not change, the 1g hide sample accurately taken is added in 10mL ml headspace bottle, 30min is balanced at 50 DEG C, insert 65 μm of PDMS/DVB fiber heads, adjustment is the position of fixed extractor head in head space volume also, in 50 DEG C of extraction 30min.
4. method according to claim 1, is characterized in that, described chromatographic condition is: chromatographic column: Agilent19091J-433-HP-5 capillary column (30m × 250 μm × 0.25 μm); Heating schedule: 60 DEG C keep 2min, and 5 DEG C/min rises to 230 DEG C, keep 20min; Carrier gas (He) flow velocity 1.0mL/min, injector temperature: 250 DEG C; Input mode: Splitless injecting samples; Desorption time: 5min.
5. method according to claim 1, is characterized in that, described Mass Spectrometry Conditions is: electronics bombardment (EI) ion gun; Electron energy 70eV; Transmission line temperature 230 DEG C; Ion source temperature 170 DEG C; Ion hydrazine temperature 150 DEG C, mass scan range
m/z30 ~ 800.
6. method according to claim 1, it is characterized in that, the method of Analysis and Identification described in step 3) is: to peak each in total ion current figure after scanning of the mass spectrum, obtain full scan mass spectrogram, resolve collection of illustrative plates and obtain related data, by carrying out qualitative, quantitative with mass spectrometric data system NIST and the comparative analysis of Willey standard diagram database to volatile constituent, determine the volatile constituent in donkey hide, horse skin or ox-hide and content.
7. method according to claim 6, is characterized in that, adopts the normalized method of integral area to determine the percentage contents of each component in volatile constituent.
8. utilize a standard for odour component discriminating donkey hide, this standard is used for the match parameters of volatile constituent and its standard that will obtain, and it is characterized in that, this standard comprises following parameter:
The peculiar volatile constituent of donkey hide comprises 16 kinds, it is 36.26% that described peculiar volatile constituent percentage contents in volatile constituent accounts for, and each component and percentage contents thereof are respectively: n-hexyl aldehyde 1.92%, enanthaldehyde 2.40%, 1-(2-hydroxy-4-methoxyphenyl) ethyl ketone 2.58%, acetic acid 5.33%, propionic acid 2.63%, butyric acid 5.23%, 2-Methyl Butyric Acid 2.61%, 3 Methylbutanoic acid 4.05%, 2-(2-Butoxyethoxy) acetate ethanol ester 0.95%; Chain hydrocarbon: 2-methyl isophthalic acid-trifluoroacetyl group pentane 0.51%, 1,1'-2-propyl group-1,3-propylidene) bicyclohexane 1.20%, eicosane 1.32%, (E)-9-eicosylene 1.28%, aromatic hydrocarbon, comprises phenol 2.4%, biphenyl 0.85%; A small amount of alcohol: (E)-2-decen-1-ol 0.99%.
9. standard according to claim 8, is characterized in that, also comprises the standard differentiating horse or ox-hide, and its parameter is as follows respectively:
The peculiar volatile constituent of horse skin comprises 14 kinds, described peculiar volatile constituent percentage contents in volatile constituent is 16.31%, each component and percentage contents thereof are respectively: 14-vaccenic acid aldehyde 3.83%, 6,10-dimethyl-2-undecyl ketone 0.45%, 2-HEPTANONE 1.49%, 5-heptyl dihydro-2(3 hydrogen)-furanone 0.72%, 2-1-methyl ethylidene cyclohexanone 1.15%, oxalic acid decyl propyl diester 2.02%, sulphurous acid hexyl octyl group ester 0.36%; Nitrogen-containing compound: 2-ethyl acridine 0.09%, 3-crotonamide 0.71%, 4-methyl-2 pentanone dimethyl hydrazone 0.12%, propionamide 0.04%, cis-3,4-dimethyl-2-phenyl tetrahydrochysene-Isosorbide-5-Nitrae-thiazine 1.75%; Unsaturated hydrocarbon: E-3-nonene 2.1%, 4-nonene 1.48%;
The peculiar volatile constituent of ox-hide comprises 8 kinds, described peculiar volatile constituent percentage contents in volatile constituent is 17.57%, and each component and percentage contents thereof are respectively: 6-methyl-Benzaldehyde,2-hydroxy 1.92%, 6-methyl-2-HEPTANONE 1.44%, (Z)-14-tricosenoic acid 4.06%, ethyl caprilate 3.52%, ethyl pelargonate 1.44%; The chloro-4-(4-methoxyphenyl of a small amount of nitrogen-containing compound: 2-)-6-(4-nitrobenzophenone) pyrimidine 1.47%; Aromatic hydrocarbon: benzepine 2.18%; Alcohol: 2-methyl-1-butene alcohol 1.54%.
10. utilize odour component to differentiate a method for donkey, horse or ox-hide, it is characterized in that, the method step is:
Testing sample is determined its volatile constituent according to the method according to any one of claim 1-7;
The volatile constituent determined in step 1) searched in parameter according to claim 8, the peculiar volatile ingredient determination testing sample according to finding is donkey hide, or
The volatile constituent determined in step 1) is carried out searching coupling in the parameter described in claim 8 or 9, and the result determination testing sample according to coupling is corresponding donkey, horse or ox-hide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107014957A (en) * | 2017-05-09 | 2017-08-04 | 东阿阿胶股份有限公司 | A kind of method of utilization odour component Quick donkey hide quality |
| CN107536850A (en) * | 2017-05-09 | 2018-01-05 | 东阿阿胶股份有限公司 | Excellent donkey-hide gelatin of a kind of odor qualities and preparation method thereof |
| CN109212059A (en) * | 2018-08-30 | 2019-01-15 | 上海应用技术大学 | A kind of detection method of automobile leather odour component |
| CN114563491A (en) * | 2022-01-14 | 2022-05-31 | 山东师范大学 | Method for monitoring quality change of sample in donkey-hide gelatin processing technology |
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