CN105784906B - Squalene differentiates the method for building up of label as olive oil and camellia seed oil - Google Patents
Squalene differentiates the method for building up of label as olive oil and camellia seed oil Download PDFInfo
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- CN105784906B CN105784906B CN201610218149.6A CN201610218149A CN105784906B CN 105784906 B CN105784906 B CN 105784906B CN 201610218149 A CN201610218149 A CN 201610218149A CN 105784906 B CN105784906 B CN 105784906B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
Differentiate the method for building up of label as olive oil and camellia seed oil the invention discloses a kind of squalene.Take squalene standard items to be made into various concentrations first, detected to obtain the peak area of various concentrations with gas chromatograph, calculate the standard curve and calculation formula of peak area and concentration relationship.Then from the camellia seed oil and olive oil extracted respectively from tea seed, olive fruit, or tank oil takes micro-example to carry out high temperature saponification processing, with petroleum ether extraction squalene, detect to obtain the peak area of squalene in sample with gas chromatograph, obtain the squalene content of various samples.Finally, Variant statistical analysis is made to the squalene content of all camellia seed oils, olive oil, draws the squalene content of camellia seed oil, olive oil.Inventive samples pre-treatment is simple, and data are intuitive and reliable, reproducible.
Description
Technical field
The present invention relates to grease detection field in food inspection, especially, is made the present invention relates to one kind with squalene content
Differentiate the gas-chromatography detection method and discrimination standard of foundation for olive oil and camellia seed oil.
Background technology
Olive oil is a kind of ancient oil kind for originating in Mediterranean, has and reduces cardiovascular and cerebrovascular disease generation, improves human body
Digestive system function, anticancer, it is anti-aging, stimulate circulation it is alive with multiple efficacies, its nutritive value such as nervous system development
Boundary gains public acceptance already, is described as " liquid golden ", " vegetable oil queen ".Camellia seed oil is carried from Theaceae tea oil tree seed
The China domestic ancient oil kind taken, its chemical property, especially aliphatic acid composition are closely similar with olive oil.Because it has prevention
Angiocardiopathy, oxidation and removing free radicals and other effects also have very high nutritive value, and camellia seed oil is described as " east olive
Oil ", " long life oil ".
China is the original producton location of oil tea, is camellia seed oil producing country maximum in the world, deep to be welcome by domestic consumer, because
Limits throughput, in recent years price be in up-trend.The olive oil of domestic market is mainly from European import.Olive oil is divided into force feed
With the class of Marc oil two of solvent extraction, olive oil is generally squeezed as edible oil, price is higher, and Marc oil is generally as industry
It is inexpensive for cosmetics and daily chemical product, feed with oil, or even it is significantly less than domestic camellia seed oil.Past Chinese market
The camellia seed oil of appearance is usually relatively low palm oil of its price etc..Gas chromatograph generally adopts in being detected with edible oil
With, by fatty acid profile and content, commonly use edible oil with it and pretend to be camellia seed oil to be easy to differentiate, it is illegal for this in recent years
Businessman starts to pretend to be camellia seed oil with fatty acid profile and ratio the import poor quality pomace olive oil similar to camellia seed oil, in Zhejiang
Jiang Shengyi is investigated and prosecuted reinstates the important case that pomace olive oil pretends to be camellia seed oil more.According to the Quzhou daily paper on the 8th of August in 2012,
The quality supervision department of city was once directed to pretends to be the illegal discreditable behavior of camellia seed oil to carry out special administration with olive Marc oil.Anhui Province
" olea europaea fruit residual oil " is once also pretended to be into camellia seed oil as investigation content in Huoshan County's focus efforts on special areas camellia seed oil activity.But so far
The present is there is not yet can effectively differentiate that olive oil pretends to be the ready-made detection method of camellia seed oil.
Existing Chinese national standard《GB11765-2003 camellia seed oils》In not on forming similar olive oil to aliphatic acid
Discrimination method, have in existing disclosed patent application and differentiate olive oil kind and olive oil quality using physical detection means
Content, such as use the olive oil fast detection method (application number of Raman spectrum characteristic peak signal intensity ratio
200810106530.9) discriminating of camellia seed oil and olive oil, and required instrument valency, but in its adulterated grease used are not referred to
Lattice are expensive, and not easy to operate, data analysis is cumbersome.The patent of camellia seed oil discriminating is related to, it is such as a kind of to differentiate oil-tea camellia seed oil
Simple and quick method (application number CN201010217382.5), according to the patent application describe, using in camellia seed oil contain steroidal into
Point, the principle that the composition and developer can develop the color distinguishes the vegetable oil that other are free of steroidal, is olive the shortcomings that this method
Olive oil and other vegetable oil for containing steroid component can not use, and chromogenic reaction is not accurate enough, can not accomplish quantitative analysis.
Relating to mix pseudo- discrimination method to camellia seed oil in document and some standards, principle used is camellia seed oil aliphatic acid composition,
Such as Yan Xiaoli, Xu Xin《Adulterated camellia seed oil Qualitive test-gas chromatography》(《Food engineering》12 phases in 2011), middle utilization
Its shortcoming of the method for such principle is to be difficult to the olive oil similar to camellia seed oil aliphatic acid composition being distinguished.Zhou Jianping
And Guo Hua《Camellia seed oil method for quantitatively determining is studied》《Chinese oil》The 2nd 55-57 pages of the phase of volume 28 in 2003 employs vinegar
Acid anhydrides-concentrated sulfuric acid colour developing hair differentiates colored complex method in camellia seed oil, but its principles of chemistry is probably the tea soap with residual
Plain phase reaction, but we carry out checking and find the method to bad to the higher camellia seed oil effect of purity, and repeatability is bad.
Zhong Donglian etc. the gas chromatography of squalene content " in camellia seed oil measure " (《Assay office》2011
104-106 pages of the o. 11ths of volume 30) in be related to squalene content in camellia seed oil measure, Geng Shuxiang etc. " different cultivars and
The detection and analysis of squalene in maturity olive oil | " (《Chinese grain and oil journal》The 2nd 123-129 pages of the phase of volume 28 in 2013) in
The measure of squalene content in olive oil is related to, but this two papers pertain only to the methodology demonstration of squalene detection, do not have
Grease differentiates related fields research contents.Long Zhenghai, kingly way put down " camellia seed oil and olive oil chemical constitution study " (《Chinese grain
Oily journal》The 2nd 121-123 pages of the phase of volume 23 in 2008) report that squalene content is apparently higher than camellia seed oil in olive oil, but its
Used sample is commodity, respectively only 1 sample size, not general not using the reliable method from former fruit extraction oil product
All over property and representative meaning, Method validation is not more done.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of squalene as olive oil and oil tea
Seed oil differentiates the method for building up of label.
The purpose of the present invention is achieved through the following technical solutions.
A kind of squalene differentiates the method for building up of label as olive oil and camellia seed oil, comprises the following steps：
(1) squalene standard items are taken, gradient solution is configured to chromatographic grade n-hexane, is determined by GC, establish standard song
Line；
(2) olive fruit is crushed, olive oil is extracted with physical squeezing method；Camellia seed oil is extracted by chemical-solvent method；
(3) microstandard olive oil or camellia seed oil are taken；The sampling amount of olive oil is 5mg, camellia seed oil 100mg；
(4) add potassium hydroxide-ethanol solution and high temperature saponification processing is carried out to sample；
(5) room temperature is cooled to, the squalene in petroleum ether extraction sample is used after addition saturated nacl aqueous solution；
(6) stratification, pure water is added after separating supernatant, is washed till neutrality；
(7) stratification, a small amount of anhydrous sodium sulfate is added after separating supernatant；
(8) centrifuged after shaking, take supernatant and dry up；
(9) add after organic solvent redissolves and cross film；The organic solvent is n-hexane, crosses 0.45 μm of organic film；
(10) the laggard GC of n-hexane redissolution is added after nitrogen drying to be detected；
(11) bring squalene peak area on gas chromatogram into standard curve and calculate squalene content；
(12) difference analysis is carried out to camellia seed oil and olive oil squalene content；
(13) using GC-MS to the appearance time of squalene in sample and standard items squalene, fragmentation pattern and chemical constitution
Compare.
The equation of linear regression that standard curve is drawn described in step (11)：Y=0.3662x-1.0791, R2=
0.9999。
In the step (11), squalene content is respectively in olive oil and camellia seed oil in olive oil, camellia seed oil
0.15 ± 0.07mg/g and 6.72 ± 2.05mg/g, p ＜ 0.01.
Potassium hydroxide-ethanol solution concentration is 2mol/L in the step (4), addition 5mL, saponification temperature 85
DEG C, saponification time 60min.
In the step (8), centrifugal speed 2000r/min, centrifugation time 5min.
The chromatographic column used in is HP-5MS (30m × 0.25mm × 0.25 μm) in the step (11), and instrument is
Agilent7890A type gas-chromatography instruments.
Described method, further GC conditions are：Carrier gas：High pure nitrogen；Injector temperature：250℃；Detector
270 DEG C of FID temperature；100 DEG C of column temperature, 2min, 15 DEG C/min is warming up to 290 DEG C, 5min；The μ L of sample size 1, split ratio 50:1.
A kind of squalene differentiates the application of label as olive oil and camellia seed oil, comprises the following steps：From treating
Take sample to carry out high temperature saponification processing in the olive oil or camellia seed oil of survey, with petroleum ether extraction squalene, use gas chromatograph
Detection obtains the peak area of squalene in testing sample, and peak area is substituted into described standard curve, obtains the angle of testing sample
Squalene content；The squalene of testing sample is compared with reference to olive oil or with reference to the squalene content in camellia seed oil, sentenced
The Species origin or the true and false of disconnected olive oil to be measured or camellia seed oil.
The beneficial effects of the invention are as follows：
(1) present invention differentiates using squalene as label to olive oil and camellia seed oil, and method is easy, general tool
The laboratory for having gas chromatograph can be carried out；
(2) this method is reproducible, reliable results, and recovery of standard addition 100%-106.3%, relative standard deviation exists
0.13%-0.81%.
(3) this method sampling amount is few, greatly reduces the loss of sample, and detection efficiency is high；
(4) this method can be to providing greatly reference currently without the unified standard for differentiating olive oil and camellia seed oil；
(5) this method directly extracts grease from raw material, greatly avoids the influence of squalene content in process
The factor artificially added.
Brief description of the drawings
With reference to specific embodiments and the drawings, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate
The present invention rather than the limitation scope of the invention.
Fig. 1 is squalene standard curve collection of illustrative plates；
Fig. 2 is that camellia seed oil is analyzed with olive oil squalene content difference；
Fig. 3 is extraction camellia seed oil GC-MS collection of illustrative plates；
Fig. 4 is squalene structural formula in extraction camellia seed oil；
Fig. 5 is fresh squeezing olive oil GC-MS collection of illustrative plates；
Fig. 6 is squalene structural formula in fresh squeezing olive oil；
Fig. 7 is squalene standard specimen GC-MS collection of illustrative plates；
Fig. 8 is squalene guide sample structure formula.
Embodiment
Instant invention demonstrates the content of squalene in a variety of self-carry and commercially available olive oil and camellia seed oil, there is provided a kind of angle
MF59 differentiates method for building up and the application of label as olive oil and camellia seed oil.The present invention uses chemical method, with more
Conventional gas chromatograph, by simple pretreatment process, can preferably separate squalene, pass through peak as detecting instrument
The comparison of area can directly make result judgement, and the standard curve established by external standard method then can be to the squalene concentration in sample
Or content is accurately calculated, so as to make accurately quantitative discriminating to olive oil and camellia seed oil, method is reproducible, data
It is intuitive and reliable.
1st, squalene standard items are taken, are configured to gradient solution, are detected with gas-chromatography instrument, pass through concentration and peak area
Relation obtains standard curve and concentration calculation formula.
2nd, extract camellia seed oil from tea seed and olive fruit and olive oil, camellia seed oil use extract by solvents, carried
It is n-hexane to take solvent, and olive oil is extracted using physical squeezing method.
3rd, micro (tea oil 100mg, olive oil 5mg) testing sample is taken in 30mL test tubes, to add 5mL 2mol/
LKOH- ethanol solutions；It is placed in 85 DEG C of water-baths after saponification 1h and removes cooling；5mL saturation NaCl solutions are added, add 4mL
Petroleum ether；Stratification after fully shaking, take supernatant in test tube, add 4mL pure water be washed to neutrality, take supernatant liquid in
In another test tube, and add a small amount of anhydrous sodium sulfate；5min is centrifuged with 2000r/min after concussion；Supernatant is shifted in new test tube
In, nitrogen is blown to no liquid；Film (the organic filter membranes of ф 13*0.45 μm) was crossed after adding 2mL n-hexanes (analysis is pure) fully dissolving；Again
Secondary nitrogen be blown to it is dry, 100 μ L n-hexanes (chromatographically pure) redissolve after carry out gas chromatographic detection.Detecting step is as follows：
4th, gas chromatographic analysis：With Agilent 7890A type gas chromatograph for determination aliphatic acid, with Agilent chemical work
Stand and gather collection of illustrative plates, and the spectral data that Treatment Analysis is gathered.Chromatographic peak is identified using squalene standard specimen.Quantitative manner
Using area-method, quantitative approach is external standard method.
5th, spectrogram acquisition process：It is qualitative using the method compareed with standard items retention time, i.e., determined according to relative retention value
Property；Using quantified by external standard method, i.e., standard curve is established by the peak area of various concentrations squalene standard sample, by testing sample
Peak area, which brings standard curve into, can calculate respective concentration.
6th, analytical conditions for gas chromatography：Chromatographic condition：HP-5MS (30m × 0.25mm × 0.25 μm) capillary column；Carrier gas：
High pure nitrogen；Injector temperature：250℃；270 DEG C of detector (FID) temperature；Column temperature 100 DEG C (2min), 15 DEG C/min are warming up to
290℃(5min)；The μ L of sample size 1, split ratio 50:1.
7th, using GC-MS to the appearance time of squalene in sample and standard items squalene, fragmentation pattern and chemical constitution ratio
It is right.GC-MS chromatographic conditions are identical with GC, and Mass Spectrometry Conditions are：Solvent delay 3.5min；Ion gun：EI；Ion source temperature：230
℃；Electron energy 70eV；MSD transmission line temperature：250℃；The qualitative ion m/z69.1 and 221.0 of squalene.
Embodiment one：Establish standard curve
Using n-hexane as solvent, compound concentration is 10mg/L-700mg/L squalene standard liquid.With squalene concentration
(mg/L) it is abscissa, corresponding peak area is that ordinate does standard curve (Fig. 1), the equation of linear regression of squalene：Y=
0.3662x-1.0791(R2=0.9999).Minimum detectability (LOD)：Using the concentration corresponding to 3 times of baseline noise as standard,
This method is 2.38 μ g/mL.
When detecting specific sample, squalene peak area in sample is substituted into regression equation can be calculated sample concentration, then
Concentration is substituted into following calculation formula, can convert to obtain corresponding content (μ g/g)：
In formula：
X：Squalene content in raw sample oil, unit are every gram of milligram (mg/g)；
Cs：Squalene content in sample introduction solution, standard curve is substituted into by squalene peak area in sample and calculates gained, unit is
Milligrams per liter (mg/L)；
V：Sample introduction overall solution volume, unit are microlitre (μ L)；
m：Testing sample sampling amount during pre-treatment, unit are gram (g).
Embodiment two：Sample collection and squalene assay
1st, tea seed and olive fruit collection and grease extraction
That is detected in the present embodiment shares 30 kinds of camellia seed oils and olive oil (table 1).Wherein numbering 1-21 tea seed
There is provided with numbering 23-26 olive fruit by Inst. of Subtropical Forestry, Chinese Academy of Forestry Sciences, tea seed derives from Zhejiang
Jinhua and Jiangxi, olive fruit derive from Sichuan Qing Chuan.
The detected sample of table 1 is detailed
By fresh olive fruit powder it is broken after extract the core, add a small amount of water, fully crush and centrifuged after stirring, supernatant is as fresh
Squeeze olive oil.Appropriate camellia seed kernel is taken to be placed in certain time in 50 DEG C of baking ovens.Room temperature is cooled to after being taken out from baking oven, it is accurate to claim
Camellia seed kernel 6g after amount drying, camellia seed kernel is shredded and is placed in glass tube, with scissors by solid-liquid ratio 1:5g/mL add just oneself
Alkane, layering is centrifuged after ultrasound on extracting 30min under the conditions of 50 DEG C of bath temperature, takes supernatant.The upper of camellia seed oil will be contained
Camellia seed oil is produced after being dried to constant weight after clear liquid revolving.
2nd, sample pre-treatments
Micro (tea oil 100mg, olive oil 5mg) testing sample is taken in 30mL test tubes, to add 5mL 2mol/
LKOH- ethanol (5.6g potassium hydroxide, 50mL absolute ethyl alcohols) solution；It is placed in 85 DEG C of water-baths after saponification 1h and removes cooling；Add
Enter 5mL saturation NaCl solutions, add 4mL petroleum ethers；Stratification after fully shaking, supernatant is taken in test tube, add 4mL
Pure water is washed to neutrality, takes supernatant liquid in another test tube, and add a small amount of anhydrous sodium sulfate；With 2000r/min after concussion
Centrifuge 5min；Supernatant is shifted in new test tube, nitrogen is blown to no liquid；Add mistake after 2mL n-hexanes (analysis is pure) fully dissolve
Cross film (0.45 μm of organic filter membrane)；Nitrogen is blown to dry again, sample introduction after 100 μ L n-hexanes (chromatographically pure) redissolve.
3rd, instrument and condition
INSTRUMENT MODEL：Agilent 7890A；Chromatographic condition：HP-5MS (30m × 0.25mm × 0.25 μm) capillary column；
Carrier gas：High pure nitrogen；Injector temperature：250℃；270 DEG C of detector (FID) temperature；Column temperature 100 DEG C (2min), 15 DEG C/min
It is warming up to 290 DEG C (5min)；The μ L of sample size 1, split ratio 50:1.
4th, testing result
The peak area of the squalene gone out after pre-treatment by gas chromatographic detection is substituted into standard curve, obtained in sample
Squalene concentration, then following calculation formula is substituted into,It can convert to obtain corresponding content (μ g/g)：
In formula：X：Squalene content in sample oil, unit are every gram of milligram (mg/g)；Cs：Squalene concentration in sample introduction solution, by sample
Middle squalene peak area substitutes into standard curve and calculates gained, and unit is milligrams per liter (mg/L)；V：Sample introduction overall solution volume, unit
For microlitre (a μ L)；m：Testing sample sampling amount during pre-treatment, unit are gram (g).
The testing result of squalene content is as shown in table 2 in 24 kinds of camellia seed oils, the inspection of squalene content in 6 kinds of olive oil
It is as shown in table 3 to survey result.
The various camellia seed oil squalene assay results of table 2
The squalene assay result of 3 various olive oil of table
5th, squalene content analysis in olive oil and camellia seed oil
Squalene content in 24 kinds of camellia seed oils and 6 kinds of olive oil is contrasted into (Fig. 2), with reference to 3 visible olive of table 2 and table
The squalene content of olive oil and camellia seed oil is respectively 6.72 ± 2.05mg/g and 0.15 ± 0.07mg/g, the squalene of olive oil
Content is 44.8 times of camellia seed oil, has significant difference (p ＜ 0.01), and this result shows that squalene is a kind of effective mirror
The label of other olive oil and camellia seed oil.
Embodiment two：Squalene mark-on reclaims
100mg camellia seed oils are taken, carry out sample pre-treatments by the description in specific implementation method, each sample is repeated 5 times.
Two parts of 100mg camellia seed oils sample is taken simultaneously, adds carry out mark-on reclaims containing 5 μ g and 10 μ g squalene standard liquid respectively
Experiment.Method precision is shown in Table 4 with the rate of recovery.As a result this method rate of recovery is indicated between 100%-106.3%, relative standard
Deviation is between 0.13%-0.81%.
Recovery testu result in the camellia seed oil of table 4
Embodiment three：GC-MS compares to squalene in sample and standard items
1st, sample pre-treatments
Micro (tea oil 100mg, olive oil 5mg) testing sample is taken in 30mL test tubes, to add 5mL 2mol/
LKOH- ethanol (5.6g potassium hydroxide, 50mL absolute ethyl alcohols) solution；It is placed in 85 DEG C of water-baths after saponification 1h and removes cooling；Add
Enter 5mL saturation NaCl solutions, add 4mL petroleum ethers；Stratification after fully shaking, supernatant is taken in test tube, add 4mL
Pure water is washed to neutrality, takes supernatant liquid in another test tube, and add a small amount of anhydrous sodium sulfate；With 2000r/min after concussion
Centrifuge 5min；Supernatant is shifted in new test tube, nitrogen is blown to no liquid；Add mistake after 2mL n-hexanes (analysis is pure) fully dissolve
Cross film (0.45 μm of organic filter membrane)；Nitrogen is blown to dry again, sample introduction after 100 μ L n-hexanes (chromatographically pure) redissolve.
2nd, instrument condition
INSTRUMENT MODEL：Agilent 6890B；Chromatographic condition：HP-5MS UI (30m × 0.25mm × 0.25 μm) superelevation is lazy
Property capillary column；Carrier gas：High-purity helium；Injector temperature：250℃；Column temperature 100 DEG C (2min), 15 DEG C/min are warming up to 290 DEG C
(5min)；The μ L of sample size 1.Mass Spectrometry Conditions：Solvent delay 3.5min；Ion gun：EI；Ion source temperature：230℃；Electron energy
70eV；MSD transmission line temperature：250℃；The qualitative ion m/z 69.1 and 221.0 of squalene.
3rd, interpretation of result
After pre-treatment, sample detects (such as Fig. 3 and Fig. 5) by GC-MS for camellia seed oil and olive oil, and in mass spectral database
Similarity highest material is squalene after data comparison.Directly enter GC-MS detections (such as Fig. 7) with squalene standard specimen, find
Retention time fits like a glove, and the mass spectrograms of squalene standard items is shown in Fig. 8, and the mass spectrogram of squalene is shown in Fig. 4 and Fig. 6 in sample.By
The retention time of squalene and standard items squalene, chemical structural formula are consistent with fragment ion figure in visible above sample.
Claims (8)
1. a kind of squalene differentiates the method for building up of label as olive oil and camellia seed oil, it is characterised in that including following
Step：
（1）Squalene standard items are taken, gradient solution is configured to chromatographic grade n-hexane, is determined by GC, establish standard curve；
（2）Olive fruit is crushed, olive oil is extracted with physical squeezing method；Camellia seed oil is extracted by chemical-solvent method；
（3）Take microstandard olive oil or camellia seed oil；The sampling amount of olive oil is 5 mg, and camellia seed oil is 100 mg；
（4）Add potassium hydroxide-ethanol solution and high temperature saponification processing is carried out to sample；
（5）Room temperature is cooled to, the squalene in petroleum ether extraction sample is used after addition saturated nacl aqueous solution；
（6）Stratification, pure water is added after separating supernatant, is washed till neutrality；
（7）Stratification, a small amount of anhydrous sodium sulfate is added after separating supernatant；
（8）Centrifuged after concussion, take supernatant and dry up；
（9）Add after organic solvent redissolves and cross film；The organic solvent is n-hexane, crosses 0.45 μm of organic film；
（10）The laggard GC of n-hexane redissolution is added after nitrogen drying to be detected；
（11）Bring squalene peak area on gas chromatogram into standard curve and calculate squalene content；
（12）Difference analysis is carried out to camellia seed oil and olive oil squalene content；
（13）The appearance time of squalene in sample and standard items squalene, fragmentation pattern and chemical constitution are compared using GC-MS.
2. the method as described in claim 1, it is characterised in that step（11）Described in the linear regression side that draws of standard curve
Journey：Y=0.3662x-1.0791, R2=0.9999。
3. the method as described in claim 1, it is characterised in that the step（11）In, olive oil in olive oil, camellia seed oil
It is respectively 0.15 ± 0.07 mg/g and 6.72 ± 2.05 mg/g with squalene Content in camellia seed oil, p ＜ 0.01.
4. the method as described in claim 1, it is characterised in that the step（4）Middle potassium hydroxide-ethanol solution concentration is 2
Mol/L, addition are 5 mL, and saponification temperature is 85 DEG C, and saponification time is 60 min.
5. the method as described in claim 1, it is characterised in that the step（8）In, centrifugal speed is 2000 r/min, from
The heart time is 5 min.
6. the method as described in claim 1, it is characterised in that the step（11）The middle chromatographic column used in is HP-5MS, instrument
Device is Agilent 7890A type gas-chromatography instruments.
7. method as claimed in claim 6, it is characterised in that GC conditions described further are：Carrier gas：High Purity Nitrogen
Gas；Injector temperature：250℃；270 DEG C of detector FID temperature；100 DEG C, 2 min, 15 DEG C/min of column temperature is warming up to 290 DEG C, and 5
min；The μ L of sample size 1, split ratio 50:1.
8. a kind of squalene as claimed in claim 1 differentiates answering for the method for building up of label as olive oil and camellia seed oil
With, it is characterised in that comprise the following steps：Sample is taken to carry out high temperature saponification processing from olive oil or camellia seed oil to be measured,
With petroleum ether extraction squalene, detect to obtain the peak area of squalene in testing sample with gas chromatograph, peak area is substituted into
Described standard curve, obtain the squalene content of testing sample；By the squalene of testing sample with referring to olive oil or reference
Squalene content in camellia seed oil compares, and judges the Species origin or the true and false of olive oil to be measured or camellia seed oil.
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| CN115010572A (en) * | 2022-07-07 | 2022-09-06 | 广州美林生态科技有限公司 | Method for extracting squalene and vitamin E |
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| CN102565217B (en) * | 2011-12-16 | 2014-04-09 | 中国农业科学院农产品加工研究所 | Method for simultaneously determining phytosterol and squalene in vegetable oil |
| CN103149303B (en) * | 2013-03-15 | 2016-03-02 | 云南省林业科学院 | The rapid assay methods of fatty acid and squalene in vegetable oil |
| CN105259293B (en) * | 2015-11-13 | 2018-09-25 | 北京出入境检验检疫局检验检疫技术中心 | Differentiate the method in the olive oil place of production based on isotope mass spectrometry technology |
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