CN103528986A - Method for identifying drainage oil based on finger-print technology - Google Patents
Method for identifying drainage oil based on finger-print technology Download PDFInfo
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- CN103528986A CN103528986A CN201210231653.1A CN201210231653A CN103528986A CN 103528986 A CN103528986 A CN 103528986A CN 201210231653 A CN201210231653 A CN 201210231653A CN 103528986 A CN103528986 A CN 103528986A
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Abstract
The invention relates to a method for identifying drainage oil based on a finger-print technology, belonging to the field of quality and safety detection of agriculture products. According to the traditional method for identifying the drainage oil, basically, traditional morphological identification and physical and chemical identification are used for identifying the authenticity of the drainage oil and evaluating the good and bad of the drainage oil, so that the traditional method has more human factors, or only concentrates on the individual component of many complex components but neglects many other components in the drainage oil. According to the method for identifying drainage oil based on the finger-print technology, infrared spectroscopy (IR), ultraviolet-visible spectrum and gas chromatography-mass spectrum (GC-MS) are respectively used for establishing a finger-print database, the fatty acid component of an oil sample to be identified is analyzed, and the drainage oil product is identified accurately by combining the result of relative degree of unsaturation (U/R) of the specificity components myristic acid and fatty acid of the drainage oil. Therefore, the problem that the drainage oil is identified only through a few single indexes but cannot be identified completely and accurately at present is solved, furthermore, the established finger-print database is easy to maintain, and the method has good identification accuracy and repeatability, and has a high practical value.
Description
Technical field
The present invention relates to the waste oil authentication technique based on fingerprint pattern technology, belong to quality of agricultural product and safety detection field.
Background technology
Waste oil is quality, health extreme difference, peroxide value, acid value, moisture, carbonyl valency, interior aldehyde, etc. the unedible oil of index severe overweight.Hogwash fat, frying oil, edible oil inferior, mix pseudo-edible wet goods and be referred to as waste oil.
It is to differentiate and the definite true and false of physics and chemistry discriminating with traditional proterties substantially that the discriminating of China's waste oil at present detects, and evaluates good and bad.The human factor of identifying is larger, or only considers the indivedual compositions in numerous complicated composition, and has ignored other all multicomponents of waste oil.Fingerprint pattern technology is Quality Control pattern and the Chinese crude drug true and false authentication technique of current internationally recognized control traditional Chinese medicine quality.Finger-print has higher intuitive, and the information of a large amount of allied compound the Nomenclature Composition and Structure of Complexes can be provided, and effectively reduces the mistake that artificial subjective judgement causes.
Summary of the invention
The object of the invention is to design a kind of waste oil authentication technique based on fingerprint pattern technology, solve traditional proterties discriminating and physics and chemistry and differentiate the problems such as artificial controllability, complicated inaccuracy.Utilize infrared spectrum
(IR), the technology such as ultraviolet-visible spectrum (UV), gas chromatography-mass spectrum (GC-MS) coupling, set up analyzing detecting method and the fingerprints database of waste oil fatty acid composition, thereby solve that current waste oil is only used several single indexs and the difficulty that cannot comprehensively accurately differentiate.
Step of the present invention is as follows:
1) by after ground KBr powder for drying compressing tablet, with suction pipe, get respectively qualified edible oil (peanut oil, rapeseed oil, mediation wet goods) and waste oil (comprising hogwash fat, frying oil, restaurant wet goods), each fine-still 1 drops on every part of pressing potassium bromide troche, utilizes infrared spectrum (IR) to scan (sweep limit 4000cm to the spectral absorption of sample
-1～400cm
-1), the infrared spectrum of setting up oil product absorbs spectrum library.
2) draw respectively qualified edible oil (peanut oil, rapeseed oil, mediation wet goods) and waste oil (comprising hogwash fat, frying oil, restaurant wet goods) to quartz colorimetric utensil, using distilled water as reference, carry out uv-visible absorption spectra scanning (sweep limit 230nm～800nm), the ultraviolet-visible spectrum of setting up oil product absorbs spectrum library.Having detected oil sample need clean cuvette with isooctane at every turn, in order to avoid sample cross pollution.
3) get respectively qualified edible oil (peanut oil, rapeseed oil, mediation wet goods) and waste oil (comprising hogwash fat, frying oil, restaurant wet goods) to 10mL color comparison tube, at room temperature carry out esterification processing.The upper solution of drawing after esterification is entered gas chromatograph-mass spectrometer (GCMS) (GC-MS), volatile organic matter in total ion current figure (TIC) is carried out to qualitative scanning (sweep limit 10-500amu) and peak area normalization quantitative test, each compound is retrieved and check analysis with NIST spectrum storehouse, sets up the gas chromatography-mass spectrum fingerprints database of corresponding oil product.
4) get that oil content to be identified does not perform step 1, step 2 and step 3, obtain respectively that infrared spectrum absorbs collection of illustrative plates, uv-visible absorption spectra absorbs the finger-prints such as collection of illustrative plates and gas chromatography-mass spectrum total ion current figure.By difference between spectrogram and data, utilize the content difference of similarity evaluation method, relative intensity pairing comparision, index components etc., various finger-print information is carried out to comprehensive distinguishing analysis, set up Quality Control pattern.
The present invention sets up multi-target ingredient and multispectral finger-print Quality Control technology and the overall evaluation system of waste oil, discriminating accuracy to waste oil is large, after infrared spectrum (IR), uv-visible absorption spectra (UV) and three kinds of fingerprints databases of gas chromatography-mass spectrum (GC-MS) are set up, be easy to safeguard and method good stability, can reuse, practical value is high.
Accompanying drawing explanation
Fig. 1 is corn oil infrared spectrogram
Fig. 2 is hogwash fat infrared spectrogram
Fig. 3 is certain blending stock uv-visible absorption spectra figure
Fig. 4 is frying oil uv-visible absorption spectra figure
Fig. 5 is gas-matter coupling total ion current figure of certain blending stock
Peak name: palmitic acid (11.56min, 13.35%), stearic acid (14.81min, 5.08%), cis-oleic acid (15.24min, 25.94%), cis-linoleic acid (15.95min, 44.71%), cis-leukotrienes (16.96min, 6.51%), positive 20 carbonic acid (17.98min, 0.49%)
Fig. 6 is oily gas-matter coupling total ion current figure for certain restaurant
Peak name: myristic acid (8.21min, 1.08%), palmitic acid (11.56min, 40.79%), stearic acid (14.81min, 6.30%), cis-oleic acid (15.24min, 38.10%), cis-linoleic acid (15.95min, 10.12%), positive 20 carbonic acid (17.98min, 0.51%)
Embodiment
Embodiment: first get oil to be measured with suction pipe, fine-still 1 drops on pressing potassium bromide troche, utilize infrared spectrum (IR) to measure infrared spectrum and absorb collection of illustrative plates, corrected oil in collection of illustrative plates and fingerprint databases and waste cooking oil collection of illustrative plates are compared, if substantially conform to certain collection of illustrative plates outline proportion in spectrum storehouse, can tentatively be judged as this oil product, yet, most of qualified edible oil and waste oil infrared spectrum contour similarity are high, only with spectrogram profile indistinguishable.For further investigating the difference of oil product infrared spectrum, specific infrared absorption peak relative intensity is compared, choose total absorption peak---the 1745cm in each grease
-1absorption peak, the stretching vibration peak absorption intensity of carbonyl (C=O) is benchmark, other specific absorption peak intensity and its relatively obtain relative intensity, relatively each oil product infrared absorption relative intensity size, and building database.Fig. 1 and Fig. 2 are respectively the infared spectrum of certain qualified corn oil and hogwash fat, due to 3008cm
-1c-H stretching vibration peak (content of unsaturated fatty acid in reflection oil product) for unsaturated carbon, found that A
3008cm-1/ A
1745cm-1ratio difference is larger, as the A of corn oil
3008cm-1/ A
1745cm-1be 0.7323, and hogwash fat is 0.5194.
Next step carries out ultraviolet-visible spectrum scanning.Due to below 230nm, the matrix interference of sample causes more greatly unstability of base line fixed, so the lower limit of spectral scan is at 230nm place.Using distilled water as reference liquid, various greases are placed in to quartz colorimetric utensil, within the scope of 230nm～800nm, carry out respectively uv-visible absorption spectroscopy scanning.From ultraviolet-visible spectrogram, the spectrogram of various greases there is some difference property.As peanut oil, blending stock, corn oil and biodiesel all start to occur absorption peak (as Fig. 3 blending stock uv absorption figure) below 400nm, and hogwash fat and frying oil go out peak position all after 400nm (Fig. 4).Absorbance at 668nm place hogwash fat and frying oil is respectively 0.195 and 0.097, all obviously be greater than qualified edible oil (between 0.002-0.012), and frying oil has obvious characteristic absorption peak (Fig. 4) at 668nm place, can differentiate and distinguish with other greases.
The oil that need are differentiated carries out gas chromatography-mass spectrum (GC-MS) and detects.Oil sample is placed in to 10mL color comparison tube, add the 1mL ether-normal hexane of 1: 1 (volume ratio), fully shake up, then add 1mL absolute methanol, fully shake up, then add 1mL 0.8mol/L KOH-methanol solution, fully shake concussion 5min left and right, add deionized water to scale, stratification, gets upper strata liquid and carries out GC-MS detection fatty acid.Scanning collection of illustrative plates is out retrieved and check analysis with NIST picture library, with areas of peak normalization method, measure the relative percentage composition of fatty acid, the data that draw and gas chromatography-mass spectrum fingerprints database are compared, observe and in oil sample to be identified, whether contain the special component of waste oil---myristic acid, as shown in gas-matter coupling total ion current figure of certain blending stock (Fig. 5) and certain restaurant use oil (Fig. 6), fatty acid percentage composition is marked in after appearance time.In addition, the saturated fatty acid content of waste oil is apparently higher than qualified edible oil, and its content of polyunsaturated fatty acid is significantly lower than vegetable edible oil, known according to experimental result, the relative degree of unsaturation (U/R) of qualified edible oil is generally greater than 2.5, therefore if grease to be identified contains myristic acid, and U/R value is less than 2.5 and can be judged to be waste oil.
By the fingerprint pattern technology coupling of above three steps, can accurately synthetic determination oil to be measured whether be waste oil.
Claims (4)
1. the infrared spectrum that adopts infrared spectrum (IR) to measure oil product to be measured absorbs collection of illustrative plates, contrasts with corrected oil collection of illustrative plates, if conform to completely with corrected oil collection of illustrative plates, and specific absorption peak intensity is (as 3008cm
-1) and 1745cm
-1total peak intensity ratio conforms to corrected oil, can tentatively be defined as corrected oil, if do not conform to or matching degree not high, need carry out the test of other two kinds of spectrum.
2. pair infrared spectrum (IR) detects doubtful problematic oil product, need carry out ultraviolet-visible spectrum judges again, as oil product to be measured starts to occur absorption peak more than 400nm, and 668nm place absorbance large (as being greater than 0.03), can preliminary judgement be waste oil.
3. the sample after infrared and ultra-violet analysis, further carry out gas chromatography-mass spectrum (GC-MS) test spectrogram satisfactory for result, by oil sample with organic solvent or mixed organic solvents (arbitrary volume ratio) and the abundant esterification of certain density potassium hydroxide-methanol solution after, get upper strata liquid and carry out GC-MS detection fatty acid, carry out the comparative analysis of total ion current figure collection of illustrative plates, high with corrected oil collection of illustrative plates consistance, not containing myristic acid, and the relative degree of unsaturation of fatty acid (U/R) is greater than 2.5 for qualified oil product, otherwise is waste oil.
4. in conjunction with the 1st to the 3rd identification result of claims, synthetic determination oil product to be measured is qualified oil product or waste oil.
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| CN104020158A (en) * | 2014-06-27 | 2014-09-03 | 宜特科技(昆山)电子有限公司 | Method for detecting qualification of to-be-detected product |
| CN105823752A (en) * | 2016-03-22 | 2016-08-03 | 武汉轻工大学 | Method for fast identifying variety of edible oil through near-infrared spectroscopy method |
| WO2020190954A1 (en) * | 2019-03-19 | 2020-09-24 | The Regents Of The University Of California | Method for characterizing and identifying substances |
| CN112378892A (en) * | 2020-10-15 | 2021-02-19 | 浙江省食品药品检验研究院 | Raman spectrum-based cosmetic authenticity nondestructive identification method |
| CN112504989A (en) * | 2020-11-10 | 2021-03-16 | 青岛海关技术中心 | Method for testing, identifying and classifying industrial fatty acid and product thereof |
| CN112730410A (en) * | 2020-12-25 | 2021-04-30 | 上海海洋大学 | Method for quickly distinguishing seafood by using spectrometry |
| CN112858201A (en) * | 2021-01-20 | 2021-05-28 | 西安电子科技大学 | White spirit identification method based on ultraviolet absorption spectrum |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104020158A (en) * | 2014-06-27 | 2014-09-03 | 宜特科技(昆山)电子有限公司 | Method for detecting qualification of to-be-detected product |
| CN105823752A (en) * | 2016-03-22 | 2016-08-03 | 武汉轻工大学 | Method for fast identifying variety of edible oil through near-infrared spectroscopy method |
| CN105823752B (en) * | 2016-03-22 | 2018-10-12 | 武汉轻工大学 | The method that near infrared spectroscopy quickly differentiates edible oil type |
| WO2020190954A1 (en) * | 2019-03-19 | 2020-09-24 | The Regents Of The University Of California | Method for characterizing and identifying substances |
| CN112378892A (en) * | 2020-10-15 | 2021-02-19 | 浙江省食品药品检验研究院 | Raman spectrum-based cosmetic authenticity nondestructive identification method |
| CN112504989A (en) * | 2020-11-10 | 2021-03-16 | 青岛海关技术中心 | Method for testing, identifying and classifying industrial fatty acid and product thereof |
| CN112730410A (en) * | 2020-12-25 | 2021-04-30 | 上海海洋大学 | Method for quickly distinguishing seafood by using spectrometry |
| CN112858201A (en) * | 2021-01-20 | 2021-05-28 | 西安电子科技大学 | White spirit identification method based on ultraviolet absorption spectrum |
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Application publication date: 20140122 |