CN107238594B - A method of detection doping soybean oil sesame oil purity - Google Patents

A method of detection doping soybean oil sesame oil purity Download PDF

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Publication number
CN107238594B
CN107238594B CN201710250893.9A CN201710250893A CN107238594B CN 107238594 B CN107238594 B CN 107238594B CN 201710250893 A CN201710250893 A CN 201710250893A CN 107238594 B CN107238594 B CN 107238594B
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peak
sesame oil
doping
oil
soybean oil
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CN107238594A (en
Inventor
吴市学
黄玲
盛琼
蒋静晓
徐晓阳
王晓杭
蔡曦
马艳
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Zhejiang Jusming Detection Co Ltd
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Zhejiang Jusming Detection Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering

Abstract

A method of detection doping soybean oil sesame oil purity, comprising the following steps: the Raman spectroscopy of measurement pure sesame oil, soybean oil first determines each middle ingredient in 1500-1800cm respectively‑1Place has characteristic peak, calculates in wave band 1500-1800cm‑1Locate the peak area S of characteristic peakx、SdAnd 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 measured, it is measured respectively in 1500-1800cm‑1Locate the peak area and peak height of characteristic peak;The relational expression being fitted between peak area and peak height ratios S/H and soybean oil doping concentration C obtains S/H=A × (1+C)2+ B, wherein 0 < C < 1, A=1.18, B=7.04;Using the Raman spectroscopy of the laser light source measurement sample sesame oil of same wavelength, determine 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;By bringing into the formula of step 3) acquisition for acquisition, the purity of tested sesame oil sample is calculated.

Description

A method of detection doping soybean oil sesame oil purity
Technical field:
This application involves grease detection fields, the especially detection of the sesame oil purity of doping soybean oil.
Background technique:
Common edible vegetable oil has corn oil, peanut oil, soybean oil, camellia oil, rapeseed oil, sunflower oil and sesame oil Deng, contained complicated component, but all comprising all kinds of nutriments such as fatty acid, vitamins, it is the important composition portion of human diet Point.In metabolic cycles, in addition to energy is provided, the nutriment that some human bodies cannot synthesize itself is additionally provided, it is such as unsaturated Fatty 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 its Fragrance and flavour, it is very popular, but since sesame oil is squeezed out by sesame Lai and the yield of sesame is relatively Low, therefore, leading to sesame oil is also the most expensive oils of price.
Just because of sesame oil low output and price are high, lead to there is illegal operation person to adulterate fraud to it in the market, reaps staggering profits, Sesame oil adulterates that phenomenon is commonplace, is relatively fewer to the measuring tool and method of sesame oil content due in the market, and real It tests room detection method and requires strongly professional, cumbersome complexity, it is difficult to promote the use of.And country there is not the purity rubric of sesame oil yet There is especially specific requirement, this is also to be difficult to detect and prevent one of the reason of doping phenomenon occurs in the market.
The main component of edible vegetable oil is fatty acid, and type has tens kinds, and fatty acid contained by many vegetable oil has Overlapping, this is also one of sesame oil doping phenomenon the reason of can occurring, adulterated in high-quality sesame oil at present soybean oil, sunflower oil compared with It is more, it will not influence the fragrance and mouthfeel of sesame oil, under the driving of high profit, illegal retailer just blends doping in this manner Sesame oil is sold to citizen, not only compromises the legitimate rights and interests of consumer, while mixing the doping of other edible oils is inexpensively low-quality Miscellaneous oil also causes potential damage to people's health.So carrying out such as quick, the accurate detection method of sesame oil edible oil Research formulates relevant professional standard or even laws and regulations suffers from positive meaning for monitoring edible oil safety.
Edible vegetable oil fat acid content, which detects relatively conventional method, at present gas chromatography (GC), gas-chromatography matter Combination method (GC-MS) and high performance liquid chromatography (HPLC) etc. are composed, but these types of method belongs to chemical analysis method, institute The equipment operation used is more complicated, needs to pre-process sample to be tested, and time-consuming for detection, is unfavorable for promoting.Currently, such as The vibrational spectrums technologies such as near infrared spectroscopy (NIR), mid-infrared light spectrometry (MIR), FTIR spectrum method, Raman spectroscopy Research applied to edible vegetable oil detection is carried out than wide.
Compared with infrared spectroscopy, the peak that Raman spectrum includes is mostly than relatively sharp;With outstanding fingerprint ability, i.e. Raman Characteristic peak is corresponding with organic molecule functional group, and the minor change at peak can reflect out the variation 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 edible vegetable oil fat acid content.
The present inventor passes through long-term experimental study, it was found that Raman map is as liquid chromatogram, in qualitative analysis Meanwhile the rule of quantitative analysis can be found in map, by finding these rules, it is quantitative that solution sesame oil purity can be found The problem of detection difficult.
Summary of the invention:
In view of the above-mentioned problems, the purpose of the present invention essentially consists in and provides one kind and do not need to handle sample, operation letter It is single, the detection method of accurately doping sesame oil purity is detected, the purity of sesame oil to be measured can be efficiently and accurately quickly detected.
Technical solution:
A method of detection doping soybean oil sesame oil purity, specific steps include:
1) Raman spectroscopy for measuring pure sesame oil, soybean oil first, determines each middle ingredient in 1500-1800cm respectively-1 Place has characteristic peak, and calculates in wave band 1500-1800cm-1Locate the peak area S of characteristic peakx、SdAnd peak height Hx、Hd
2) the doping sesame oil of 1%, 5%, 10%, 15%, 20% and 25% soybean oil of configuration doping, and using step 1) Condition measures the Raman spectroscopy of each sample, measures it respectively in 1500-1800cm-1Locate the peak area and peak of characteristic peak It is high;
3) using between Partial Least Squares 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) using the Raman spectroscopy of the laser light source measurement sample sesame oil of same wavelength, determine it in 1500-- 1800 cm-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) bringing into acquisition in the formula of step 3) acquisition, is calculated the purity of tested sesame oil sample.
Preferably, the measurement light source uses the incident laser light source of 532nm wavelength.
Preferably, first the Raman spectrum of sample is compared with the Raman spectrum of pure sesame oil before step 5), if two Person's overlapping, then illustrate not adulterate, if not being overlapped, continues the 5) step.
The utility model has the advantages that
Compared with prior art, the present invention having following technical effect that
(1) prior art search method is cumbersome, and step is more, and time-consuming consumption material consumption power also brings pollution using chemical reagent, As long as after this method has measured standard parameter, detecting simple and convenient, efficiently and accurately;
(2) present invention has selected Raman spectrum, and 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 does not have to be handled, and directly detects, and can carry out mass Detection is worth further genralrlization into actual life.
Detailed description of the invention:
The Raman spectrogram of Fig. 1, soybean oil (1) and sesame oil (2);
The Raman spectrogram of Fig. 2,1 sample of embodiment;
The Raman spectrogram of Fig. 3,2 sample of embodiment.
Drawing reference numeral
1. soybean oil, 2. sesame oil.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated.
As shown in Fig. 1-Fig. 3, the present invention provides a kind of methods of detection 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 first, uses Metrohm MIRA Raman spectrometer measures the Raman spectroscopy of above-mentioned six samples under 532nm incident light source, respectively Determine each middle ingredient in 1500-1800cm-1Place has characteristic peak, and calculates in wave band 1500-1800cm-1Locate characteristic peak Peak area S1-S6And peak height H1-H6;And the Raman spectroscopy of each sample is measured using the condition of step 1), it surveys respectively It is determined in 1500-1800cm-1Locate the peak area and peak height of characteristic peak;
The pass between peak area and 1 doping concentration C of peak height ratios S/H and soybean oil is fitted using Partial Least Squares principle It is formula, obtains S/H=1.18 (1+C)2+ 7.04, R=0.995;
2) measure sample: the doping sesame oil 2 of configuration 5% soybean oil 1 of doping measures its Raman light according to above-mentioned same procedure It composes spectrogram (referring to fig. 2), and calculates in wave band 1500-1800cm-1Locate the peak area S=107.54 and peak height H=of characteristic peak 12.9;It brings above-mentioned formula into and calculates to obtain 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 measures its Raman light according to above-mentioned same procedure It composes spectrogram (referring to Fig. 3), and calculates in wave band 1500-1800cm-1Locate the peak area S=115.2 and peak height H=of characteristic peak 13.6;It brings above-mentioned formula into and calculates to obtain C=9.94%, error 0.6%.
Above-described embodiment is the description of the invention, is not limitation of the invention, any pair of simple transformation of the invention Structure afterwards all belongs to the scope of protection of the present invention.It should be pointed out that for those of ordinary skill in the art, can also do Many variations and modifications out;All modifications or improvement are regarded as protection scope of the present invention.

Claims (3)

1. a kind of method of detection doping soybean oil sesame oil purity, which comprises the following steps:
1) Raman spectroscopy for measuring pure sesame oil, soybean oil first, determines each middle ingredient in 1500-1800cm respectively-1Place's tool There is characteristic peak, and calculates in wave band 1500-1800cm-1Locate the peak area S of characteristic peakx、SdAnd peak height Hx、Hd
2) the doping sesame oil of 1%, 5%, 10%, 15%, 20% and 25% soybean oil of configuration doping, and using the condition of step 1) The Raman spectroscopy of each sample is measured, measures it respectively in 1500-1800cm-1Locate the peak area and peak height of characteristic peak;
3) relationship between Partial Least Squares principle fitting peak area and peak height ratios S/H and soybean oil doping concentration C is utilized Formula obtains S/H=A × (1+C)2+ B, wherein 0 < C < 1, A=1.18, B=7.04;
4) using the Raman spectroscopy of the laser light source measurement sample sesame oil of same wavelength, determine 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) bringing into acquisition in the formula of step 3) acquisition, is calculated the purity of tested sesame oil sample.
2. the method for detection doping soybean oil sesame oil purity according to claim 1, which is characterized in that measure the 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, which is characterized in that before step 5) The Raman spectrum of sample is compared with the Raman spectrum of pure sesame oil first, if the two is overlapped, illustrates not adulterate, if not weighing It is folded, then continue the 5) step.
CN201710250893.9A 2017-04-13 2017-04-13 A method of detection doping soybean oil sesame oil purity Active CN107238594B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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
CN105758836A (en) * 2016-02-18 2016-07-13 安徽芯核防务装备技术股份有限公司 Raman spectrum real-time and quantitive analysis method based on area method
CN105954258A (en) * 2016-05-26 2016-09-21 伯格森(北京)科技有限公司 Detector and detection method for edible oil doped with inferior 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