CN107238594A - A kind of method for detecting doping soybean oil sesame oil purity - Google Patents
A kind of method for detecting doping soybean oil sesame oil purity Download PDFInfo
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- CN107238594A CN107238594A CN201710250893.9A CN201710250893A CN107238594A CN 107238594 A CN107238594 A CN 107238594A CN 201710250893 A CN201710250893 A CN 201710250893A CN 107238594 A CN107238594 A CN 107238594A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
A kind of method for detecting doping soybean oil sesame oil purity, comprises the following steps：Measurement pure sesame oil, the Raman spectroscopy of soybean oil, determine each middle composition in 1500 1800cm respectively first‑1Place has characteristic peak, calculates in the 1800cm of wave band 1500‑1Locate the peak area S of characteristic peakx、Sd, and peak height Hx、Hd；The doping sesame oil of configuration 1%, 5%, 10%, 15%, 20% and 25% soybean oil of doping, and the Raman spectroscopy of each sample is determined, it is determined respectively in 1500 1800cm‑1Locate the peak area and peak height of characteristic peak；The relational expression between peak area square and peak height ratios S/H and soybean oil doping concentration C is fitted, S/H=A × (1+C) is obtained2+ B, wherein 0 ＜ C ＜ 1, A=1.18, B=7.04；The Raman spectroscopy of sample sesame oil is measured using the LASER Light Source of same wavelength, determines it in 1500 1800cm‑1The characteristic peak at place, and measure its peak area SsWith peak height Hs, obtain the ratio between its peak area and peak height Ss/Hs；Bring acquisition into step 3) obtain formula in, calculate the purity of tested sesame oil sample.
Description
Technical field：
The application is related to grease detection field, the detection of the sesame oil purity for the soybean oil that especially adulterates.
Background technology：
Conventional edible vegetable oil has corn oil, peanut oil, soybean oil, camellia oil, rapeseed oil, sunflower oil and sesame oil
Deng, contained complicated component, but be the important composition portion of human diet all comprising all kinds of nutriments such as aliphatic acid, vitamins
Point.In metabolic cycles, in addition to energy is provided, the nutriment that some human bodies can not be synthesized itself is additionally provided, it is such as unsaturated
Aliphatic acid and fat-soluble vitamin.Wherein sesame oil is edible oil the most precious in numerous vegetable oil, and sesame oil is unique due to it
Fragrance and flavour, it is very popular, but because sesame oil is by sesame is squeezed out Lai and the yield of sesame is relatively
Low, therefore, it is also price most expensive oils to cause sesame oil.
Just because of sesame oil yields poorly and price is high, cause in the market to there is illegal operation person to be adulterated to it fraud, reap staggering profits,
Sesame oil doping phenomenon is of common occurrence, is due to that the survey tool and method to sesame oil content of in the market are relatively fewer, and in fact
Test room detection method and require strongly professional, cumbersome complexity, it is difficult to promote the use of.And country does not have to the purity rubric of sesame oil yet
There is especially specific requirement, this is also that in the market is difficult to detect and prevents one of the reason for doping phenomenon occurs.
The main component of edible vegetable oil is aliphatic acid, and species has tens kinds, and the aliphatic acid contained by many vegetable oil has
Overlapping, this is also sesame oil doping phenomenon one of the reason for can occur, adulterated at present in high-quality sesame oil soybean oil, sunflower oil compared with
It is many, the fragrance and mouthfeel of sesame oil are not interfered with, under the driving of high profit, illegal retailer just adopts blends doping in such a way
Sesame oil is sold to citizen, not only compromises the legitimate rights and interests of consumer, while inexpensively low-quality mix of being adulterated to other edible oils
Health of the miscellaneous oil also to people causes potential infringement.So carrying out as the edible oils such as sesame oil are quick, accurate detection method
Research, for monitoring edible oil safety, the professional standard or even laws and regulations for formulating correlation suffer from positive meaning.
The current fatty acid content of edible vegetable oil detects that relatively conventional method has gas chromatography (GC), gas-chromatography matter
Combination method (GC-MS), and high performance liquid chromatography (HPLC) etc. are composed, but this several method belongs to chemical analysis method, institute
The equipment operation used is more complicated, and, it is necessary to be pre-processed to testing sample, time-consuming for detection, is unfavorable for promoting.At present, such as
The vibrational spectrum technologies such as near infrared spectroscopy (NIR), mid-infrared light spectrometry (MIR), FTIR spectrum method, Raman spectroscopy
Carry out applied to the research that edible vegetable oil is detected than wide.
Compared with infrared spectrum, the peak that Raman spectrum is included is mostly than relatively sharp；With outstanding fingerprint ability, i.e. Raman
Characteristic peak is corresponding with organic molecule functional group, and the minor variations at peak can reflect the change of each fatty acid composition content.Due to
Difference between edible vegetable oil fat acid is mainly the difference of carbon-carbon double bond (C=C) quantity, and non-polar group (C=C)
Raman active it is very strong, therefore Raman spectrum is relatively specific for the detection of the fatty acid content of edible vegetable oil.
The present inventor passes through long-term experimental study, it was found that Raman collection of illustrative plates is as liquid chromatogram, in qualitative analysis
Meanwhile, the rule of quantitative analysis can be found in collection of illustrative plates, by finding these rules, solution sesame oil purity can be found and quantified
The problem of detection difficult.
The content of the invention：
Sample need not be handled in view of the above-mentioned problems, the purpose of the present invention essentially consists in offer one kind, operation letter
Single, the detection method of the accurate doping sesame oil purity of detection can efficiently and accurately be quickly detected the purity of sesame oil to be measured.
Technical scheme：
A kind of method for detecting doping soybean oil sesame oil purity, its specific steps include：
1) pure sesame oil, the Raman spectroscopy of soybean oil are measured first, determine each middle composition in 1500-1800cm respectively-1
Place has characteristic peak, and calculates in wave band 1500-1800cm-1Locate the peak area S of characteristic peakx、Sd, and peak height Hx、Hd；
2) the doping sesame oil of 1%, 5%, 10%, 15%, 20% and 25% soybean oil of configuration doping, and use step 1)
Condition determines the Raman spectroscopy of each sample, and it is determined respectively in 1500-1800cm-1Locate the peak area and peak of characteristic peak
It is high；
3) using between PLS principle fitting peak area and peak height ratios S/H and soybean oil doping concentration C
Relational expression, obtains S/H=A × (1+C)2+ B, wherein 0 ＜ C ＜ 1, A=1.18, B=1.04, R=0.995；
4) Raman spectroscopy of sample sesame oil is measured using the LASER Light Source of same wavelength, determines it in 1500--
1800cm-1The characteristic peak at place, and measure its peak area SsWith peak height Hs, obtain the product SH of its peak area and peak heights；
5) bring acquisition into step 3) obtain formula in, calculate the purity of tested sesame oil sample.
It is preferred that, the measurement light source uses the incident laser light source of 532nm wavelength.
It is preferred that, in step 5) first the Raman spectrum of the Raman spectrum of sample and pure sesame oil is compared before, if two
Person is overlapping, then illustrates not adulterate, if not overlapping, proceeds the 5) step.
Beneficial effect：
The present invention compared with prior art, with following technique effect：
(1) prior art search method is cumbersome, and step is more, takes consumption material consumption power, pollution is also brought using chemical reagent,
As long as this method has been measured after canonical parameter, simple and convenient, efficiently and accurately is detected；
(2) present invention have selected Raman spectrum, and its spectral purity is high, and intensity is good, and noise is low, and testing result is accurate；
(3) this this method has universality, and sample is without being handled, and directly detects, it is possible to carry out mass
Detection, is worth further genralrlization into actual life.
Brief description of the drawings：
Fig. 1, soybean oil (1) and sesame oil (2) Raman spectrogram；
Fig. 2, the sample of embodiment 1 Raman spectrogram；
Fig. 3, the sample of embodiment 2 Raman spectrogram.
Drawing reference numeral
1. soybean oil, 2. sesame oil.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated.
As shown in Fig. 1-Fig. 3, the invention provides a kind of method for detecting doping soybean oil sesame oil purity, including following reality
Apply example.
Embodiment 1
1) equation regression：
The doping sesame oil 2 of 1%, 5%, 10%, 15%, 20% and 25% soybean oil 1 of configuration doping, is used first
Metrohm MIRA Raman spectrometers, measure the Raman spectroscopy of above-mentioned six samples under 532nm incident light sources, true respectively
Fixed each middle composition is in 1500-1800cm-1Place has characteristic peak, and calculates in wave band 1500-1800cm-1Locate the peak of characteristic peak
Area S1-S6, and peak height H1-H6；And use step 1) condition determine the Raman spectroscopy of each sample, determine respectively
It is in 1500-1800cm-1Locate the peak area and peak height of characteristic peak；
It is fitted using PLS principle between peak area square and peak height ratios S/H and the doping concentration C of soybean oil 1
Relational expression, obtain S/H=1.18 (1+C)2+ 7.04, R=0.995；
2) sample is measured：The doping sesame oil 2 of configuration 5% soybean oil 1 of doping, its Raman light is measured according to above-mentioned same procedure
Spectrogram (referring to Fig. 2) is composed, and is calculated in wave band 1500-1800cm-1Locate the peak area S ,=107.54 and peak height H=of characteristic peak
12.9；Bring above-mentioned formula into and calculate C=4.96%, error 0.8%.
Embodiment 2
1) equation regression uses the equation of embodiment 1
Measure sample：The doping sesame oil 2 of configuration 10% soybean oil 1 of doping, its Raman light is measured according to above-mentioned same procedure
Spectrogram (referring to Fig. 3) is composed, and is calculated in wave band 1500-1800cm-1Locate the peak area S ,=115.2 and peak height H=of characteristic peak
13.6；Bring above-mentioned formula into and calculate C=9.94%, error 0.6%.
Above-described embodiment is the description of the invention, is not limitation of the invention, any simple transformation to the present invention
Structure afterwards belongs to protection scope of the present invention.It should be pointed out that for the person of ordinary skill of the art, can also do
Go out many variations and modifications；All modifications or improvement are regarded as protection scope of the present invention.
Claims (3)
1. a kind of method for detecting doping soybean oil sesame oil purity, it is characterised in that comprise the following steps：
1) pure sesame oil, the Raman spectroscopy of soybean oil are measured first, determine each middle composition in 1500-1800cm respectively-1Place's tool
There is characteristic peak, and calculate in wave band 1500-1800cm-1Locate the peak area S of characteristic peakx、Sd, and peak height Hx、Hd；
2) configuration doping 1%, 5%, 10%, 15%, 20% and 25% soybean oil doping sesame oil, and use step 1) condition
The Raman spectroscopy of each sample is determined, it is determined respectively in 1500-1800cm-1Locate the peak area and peak height of characteristic peak；
3) using between PLS principle fitting peak area square and peak height ratios S/H and soybean oil doping concentration C
Relational expression, obtains S/H=A × (1+C)2+ B, wherein 0 ＜ C ＜ 1, A=1.18, B=7.04；
4) Raman spectroscopy of sample sesame oil is measured using the LASER Light Source of same wavelength, determines it in 1500--
1800cm-1The characteristic peak at place, and measure its peak area SsWith peak height Hs, obtain the ratio between its peak area and peak height Ss/Hs；
5) bring acquisition into step 3) obtain formula in, calculate the purity of tested sesame oil sample.
2. the method for detection doping soybean oil sesame oil purity according to claim 1, it is characterised in that the measurement light source
Using the incident laser light source of 532nm wavelength.
3. the method for detection doping soybean oil sesame oil purity according to claim 1, it is characterised in that in step 5) before
First the Raman spectrum of the Raman spectrum of sample and pure sesame oil is compared, if the two is overlapping, illustrates not adulterate, if not weighing
It is folded, then proceed the 5) step.
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| GR20070100763A (en) * | 2007-11-23 | 2009-06-12 | Chiesi Farmaceutici Spa | Method for determining the polymorph purity of manidipine hydrochloride. |
| CN101470077A (en) * | 2008-05-14 | 2009-07-01 | 中国检验检疫科学研究院 | Olive oil fast detection method adopting Raman spectrum characteristic peak signal intensity ratio |
| CN103512990A (en) * | 2012-06-30 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for identifying plant-derived waste oil by adopting trace fatty acid |
| CN105548377A (en) * | 2015-12-02 | 2016-05-04 | 中国石油天然气股份有限公司 | Method and apparatus for judging productive layer of crude oil |
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Denomination of invention: A method for detecting the purity of doped soybean oil sesame oil Effective date of registration: 20210915 Granted publication date: 20191115 Pledgee: Ningbo Zhenhai Rural Commercial Bank Co.,Ltd. Development Zone sub branch Pledgor: ZHEJIANG ZHENGMING TESTING Co.,Ltd. Registration number: Y2021330001618 |