CN102262067A - Attenuate total reflection infrared spectrometry for fast detection of iodine value of edible oil - Google Patents
Attenuate total reflection infrared spectrometry for fast detection of iodine value of edible oil Download PDFInfo
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- CN102262067A CN102262067A CN2010101869726A CN201010186972A CN102262067A CN 102262067 A CN102262067 A CN 102262067A CN 2010101869726 A CN2010101869726 A CN 2010101869726A CN 201010186972 A CN201010186972 A CN 201010186972A CN 102262067 A CN102262067 A CN 102262067A
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- edible oil
- infrared
- total reflection
- iodine number
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- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 34
- 239000011630 iodine Substances 0.000 title claims abstract description 34
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000008157 edible vegetable oil Substances 0.000 title claims abstract description 26
- 238000004566 IR spectroscopy Methods 0.000 title claims abstract description 6
- 238000001514 detection method Methods 0.000 title abstract description 5
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- 238000005102 attenuated total reflection Methods 0.000 claims description 15
- 230000005477 standard model Effects 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002835 absorbance Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical group [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052805 deuterium Inorganic materials 0.000 claims description 2
- XKUKSGPZAADMRA-UHFFFAOYSA-N glycyl-glycyl-glycine Natural products NCC(=O)NCC(=O)NCC(O)=O XKUKSGPZAADMRA-UHFFFAOYSA-N 0.000 claims description 2
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 2
- DGJPPCSCQOIWCP-UHFFFAOYSA-N cadmium mercury Chemical compound [Cd].[Hg] DGJPPCSCQOIWCP-UHFFFAOYSA-N 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 2
- 238000004364 calculation method Methods 0.000 description 3
- 239000004006 olive oil Substances 0.000 description 3
- 235000008390 olive oil Nutrition 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 239000010495 camellia oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention provides an attenuate total reflection infrared spectrometry for fast detection of iodine value of edible oil, comprising the following steps: A, establishing a standard curve: using seven edible oil with different iodine values as standard samples, collecting attenuate total reflection infrared spectrums of the samples, using the detected iodine values obtained by iodometry as standard values to establish the standard curve; and B, detecting a sample: carrying out infrared spectrum test on an edible oil sample to be detected under the same condition with the standard samples to obtain infrared spectrogram of the detected sample, measuring the peak area of the characteristic absorption peak, so as to obtain the iodine value of the sample according to the standard curve. The method is used for the detection of iodine value of edible oil with rapidness and accuracy, has a good application prospect, and can be widely used in the technical field of food detection.
Description
Technical field
The present invention relates to a kind of attenuated total reflection infra-red sepectrometry of fast measuring edible oil iodine number, belong to the Infrared Spectrum Technology field.
Background technology
Iodine number is the index of measure oil degree of unsaturation, is the important evidence of estimating the food plant oil quality.Assay method commonly used mainly contains vapor-phase chromatography and chemical titration (iodimetric titration).Iodimetric titration is the method that adopts in the present edible oil determination of iodine value national standard (GB/T 5532-1995, the vegetable oil iodine value is measured), the iodometric determination result accurately and reliably, but required time is long, reagent corrosivity is strong, the human factor influence is big.Advantages such as that vapor-phase chromatography has is highly sensitive, amount of samples is few, but need be with the vegetable oil esterification, required time is long, esterification effectiveness affects mensuration precision.The present invention utilizes FFIR to set up a kind of determination of iodine value of edible oil fast method in conjunction with Technique of Attenuated Total Reflectance.Compared with prior art, outstanding feature of the present invention has: 1. quick, the minute of each sample only needs 2～4 minutes; 2. accurate, relative standard deviation is less than 3%; 3. convenient, sample does not need any pre-treatment; 4. do not use and contain toxicity and corrosive reagents.
Summary of the invention
The present invention seeks to set up a kind of infrared spectrum analysis of measuring the edible oil iodine number accurately, fast and easily, thereby reach the purpose of the quick differentiation edible oil true and false.The present invention reaches the fast measuring of edible oil iodine number as follows:
A, set up typical curve
As standard model, gather its attenuated total reflection infrared spectrum with the different seven kinds of edible oils of iodine number, measure 3040cm
-1-2990cm
-1The area of infrared absorption peak in the scope, baseline is selected 3040cm
-1-2990cm
-1The iodine number of iodometric determination is set up typical curve as standard value.
B, test sample
Get identical with the standard model respectively condition of edible oil sample to be detected and carry out examination of infrared spectrum, obtain the infrared spectrogram of test sample.Measure 3008cm
-1The peak area of characteristic absorption peak, and obtain the iodine number of sample by typical curve.
Method of infrared spectrophotometry is launched in the decay of described edible oil iodine number fast measuring entirely, and concrete technical scheme comprises the steps:
A-1, infrared spectrum acquisition condition:
Detecting instrument is for being equipped with the infrared spectrometer of attenuated total reflection annex, and detecting device is DTGS detecting device or MCT detecting device, and the attenuated total reflection crystal is ZnSe; With air as a setting, same sample different incidence angles degree adopts same background; Edible oil sample to be measured is paved with the liquid tank on the ZnSe crystal of attenuated total reflection annex, the infrared spectrum of collected specimens; Same sample collecting 6 times; Clean sample cell with ethanol after collection is finished, and under infrared lamp, dry;
Sweep limit: 4000-600cm
-1
Scanning times: 32 times;
Resolution: 4cm
-1
Incident angle: 40 °, 45 °, 50 °, 55 °, 60 °, 65 °;
Operating temperature: 18-25 ℃.
The mensuration of A-2, absorbance:
The present invention selects 3008cm
-1C-H stretching vibration peak on place's carbon-to-carbon double bond is measured 3040cm as quantitative peak
-1-2990cm
-1The peak area of infrared spectrum in the scope, baseline is 3040cm
-1-2990cm
-1
B, get identical with the standard model respectively condition of commercially available edible oil sample and carry out examination of infrared spectrum, obtain the infrared spectrogram of test sample.The peak area of measurement features absorption peak, and obtain the iodine number of sample by typical curve.
Description of drawings:
Fig. 1: the attenuated total reflection Fourier of typical edible oil changes infrared spectrogram.
Fig. 2: A
3008-iodine number typical curve.
Embodiment
1, the foundation of typical curve
As standard items, set up typical curve with 7 kinds of edible oils (being followed successively by: olive oil, tea-seed oil, peanut oil, sesame oil, corn oil, soybean oil, safflower seed oil) of iodine number scope between 82 to 142:
Use silent generation that 8700 type Fourier transformation infrared spectrometers, deuterium thiosulfuric acid triglycine detecting device, Pike ATR MAX II variable-angle MATR annex, the ZnSe crystal of flying of match;
Pipette the liquid tank of edible oil sample on the ZnSe of attenuated total reflection annex crystal with suction pipe, make sample be paved with the bottom of liquid tank, the infrared spectrum of collected specimens, each sample repeated acquisition 6 times;
Instrument condition:
Sweep limit: 4000-600cm-1;
Scanning times: 32 times;
Resolution: 4cm-1;
Incident angle: 40 °, 45 °, 50 °, 55 °, 60 °, 65 °;
Operating temperature: 18-25 ℃.
The iodine number of standard model is according to the iodometric determination of GB/T 5532-1995 regulation;
Measure 3040cm
-1-2990cm
-1The peak area of infrared spectrum in the scope, baseline is 3040cm
-1-2990cm
-1
With the peak area and the iodine number drawing standard curve of standard model, and calculate equation of linear regression.
2, sample detection
Measure the infrared spectrum of testing sample respectively with the same terms of above-mentioned bioassay standard product, measure 3040cm
-1-2990cm
-1The peak area of infrared spectrum in the scope is calculated the iodine number of testing sample by typical curve.
3, methodological investigation
(1) precision test: get a duplicate samples METHOD FOR CONTINUOUS DETERMINATION 4～6 times, the relative standard deviation of result of calculation＜3% shows that instrument precision is good.
(2) stability test: get same duplicate samples, measured its iodine number at 2 hours, 4 hours, 8 hours, 12 hours and 24 hours respectively, the relative standard deviation of result of calculation＜3% shows in 24 hours stable.
(3) reappearance test: get six duplicate samples, measure its iodine number respectively, the relative standard deviation of result of calculation＜3% shows that method has reappearance preferably.
Listed examples of the present invention is intended to further illustrate the concrete operations that utilize the full emission of decay infrared spectrum fast measuring iodine number, and scope of the present invention is not constituted any restriction.
The result of several Various Edible embodiment of table 1.
| Kind | Sample number | Absorbance | Iodine number | RSD |
| Olive oil (1#) | 1 2 3 4 | 0.0110 0.0111 0.0109 0.0109 | 85.473 86.003 84.943 84.943 | 0.59％ |
| Olive oil (3#) | 1 2 3 4 | 0.0109 0.0107 0.0109 0.0110 | 84.943 83.883 84.943 85.473 | 0.79％ |
| Sunflower |
1 2 3 4 | 0.0172 0.0176 0.0173 0.0169 | 118.328 120.447 118.857 116.738 | 1.29％ |
Claims (2)
1. the attenuated total reflection method of infrared spectrophotometry of an edible oil iodine number fast measuring is characterized in that comprising the steps:
A, set up typical curve
As standard model, gather its attenuated total reflection infrared spectrum with the different seven kinds of edible oils of iodine number, the iodine number of iodometric determination is set up typical curve as standard value.
B, test sample
Get identical with the standard model respectively condition of edible oil sample to be detected and carry out examination of infrared spectrum, obtain the infrared spectrogram of test sample.The peak area of measurement features absorption peak, and obtain the iodine number of sample by typical curve.
2. according to the attenuated total reflection method of infrared spectrophotometry of the described edible oil iodine number of claim one fast measuring, its feature comprises the steps:
A-1, infrared spectrum acquisition condition:
Detecting instrument is for being equipped with the infrared spectrometer of attenuated total reflection annex, and detecting device is deuterium thiosulfuric acid triglycine detecting device (DTGS) or mercury cadmium single detecting device (MCT), and the attenuated total reflection crystal is ZnSe; With air as a setting, same sample different incidence angles degree adopts same background; Edible oil sample to be measured is paved with the liquid tank on the ZnSe crystal of attenuated total reflection annex, the infrared spectrum of collected specimens; Same sample collecting 6 times; Clean sample cell with ethanol after collection is finished, and under infrared lamp, dry;
Sweep limit: 4000-600cm
-1
Scanning times: 32 times;
Resolution: 4cm
-1
Incident angle: 40 °, 45 °, 50 °, 55 °, 60 °, 65 °;
Operating temperature: 18-25 ℃.
The mensuration of A-2, absorbance:
Select 3008cm
-1C-H stretching vibration peak on place's carbon-to-carbon double bond is measured 3040cm as quantitative peak
-1-2990cm
-1The area of infrared absorption peak in the scope, baseline is 3040cm
-1-2990cm
-1The relative standard deviation that same sample is repeatedly measured＜3%;
B, get identical with the standard model respectively condition of commercially available edible oil sample and carry out examination of infrared spectrum, obtain the infrared spectrogram of test sample.The peak area of measurement features absorption peak, and obtain the iodine number of sample by typical curve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101869726A CN102262067A (en) | 2010-05-31 | 2010-05-31 | Attenuate total reflection infrared spectrometry for fast detection of iodine value of edible oil |
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|---|---|---|---|
| CN2010101869726A CN102262067A (en) | 2010-05-31 | 2010-05-31 | Attenuate total reflection infrared spectrometry for fast detection of iodine value of edible oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424643A (en) * | 2015-12-31 | 2016-03-23 | 首钢总公司 | Method for determining content percentage in mixed oil product |
| CN107328742A (en) * | 2017-07-31 | 2017-11-07 | 国网山东省电力公司电力科学研究院 | The method of Fourier transformation decay total reflection light analysis of spectrum silane coupler percent hydrolysis |
| CN109164060A (en) * | 2018-10-08 | 2019-01-08 | 厦门卓越生物质能源有限公司 | The near infrared ray method of biodiesel iodine number |
| CN111398210A (en) * | 2020-04-22 | 2020-07-10 | 青岛市产品质量监督检验研究院 | Method for rapidly measuring urea content in automotive urea solution by utilizing mid-infrared spectrum technology |
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| WO2006011487A1 (en) * | 2004-07-30 | 2006-02-02 | National University Corporation Chiba University | Method for measuring glucose concentration in blood using infrared spectroscopy and instrument employing it |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424643A (en) * | 2015-12-31 | 2016-03-23 | 首钢总公司 | Method for determining content percentage in mixed oil product |
| CN107328742A (en) * | 2017-07-31 | 2017-11-07 | 国网山东省电力公司电力科学研究院 | The method of Fourier transformation decay total reflection light analysis of spectrum silane coupler percent hydrolysis |
| CN109164060A (en) * | 2018-10-08 | 2019-01-08 | 厦门卓越生物质能源有限公司 | The near infrared ray method of biodiesel iodine number |
| CN111398210A (en) * | 2020-04-22 | 2020-07-10 | 青岛市产品质量监督检验研究院 | Method for rapidly measuring urea content in automotive urea solution by utilizing mid-infrared spectrum technology |
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Application publication date: 20111130 |