CN100437094C - Method for fast detecting low-content mineral oil in edible oil and fat - Google Patents
Method for fast detecting low-content mineral oil in edible oil and fat Download PDFInfo
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- CN100437094C CN100437094C CNB2005100485145A CN200510048514A CN100437094C CN 100437094 C CN100437094 C CN 100437094C CN B2005100485145 A CNB2005100485145 A CN B2005100485145A CN 200510048514 A CN200510048514 A CN 200510048514A CN 100437094 C CN100437094 C CN 100437094C
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Abstract
The present invention relates to a method for fast detecting low-content mineral oil in edible oil and fat, which comprises the following steps: step 1, 0.1 to 2 ml of an oil sample to be detected is taken and added with a strong alkali solution for mixing in a container, and the strong alkali solution has the same volume and has the concentration of more than 60%; step 2, more than 95% of ethanol which has the volume of 20 to 40 times of the mixed solution is added in the mixed solution; step 3, the container is placed in a hot water bath at a temperature of 80 DEG C. to 100 DEG C. for heating and oscillation; step 4, boiling water is added for judging whether the mineral oil is contained through visual inspection by using the turbidity of the solution as a criterion. Compared with the prior art, the present invention has the advantages of The present invention has the advantages of simple and low cost of test instruments, simple and convenient operation without needing a backflow process; the present invention also has the advantages of accurate sample identification, good repeatability and easily and accurately judgement that whether the mineral oil is mixed in the oil. By overcoming the defects of a traditional experimental method, such as time and labor waste, etc. in detecting the mineral oil, the present invention can be conveniently used for the supervision and the management of a production field and a selling field of the edible oil and fat. The method can also quantitatively detect the low-content mineral oil in the edible oil and fat.
Description
Technical field
The present invention relates to grease class content detecting method, the method for quick of low content mineral oil in particularly a kind of edible oil and fat utilizes this method to identify fast and whether contains mineral oil and low content mineral oil content in the edible oil and fat.
Background technology
Edible oil and fat are happened occasionally by the quality accident that mineral oil such as industrial gasoline, kerosene, diesel oil pollute.Through investigation, the reason that pollutes has: used No. 6 solvent oils that polluted by mineral oil in grease processing; Use has the oil drum dress edible oil of residual minerals oil; The people is for mixing reasons such as puppet.
Mineral oil mainly is meant the oil substances that paraffin, whiteruss, white oil etc. extract from oil, the edible oil that edible mineral oil pollutes will work the mischief to health.Medical information is introduced: this mineral oil that can only be used in accordance with regulations in the industry, and after being eaten by mistake by human body, the injury that human body is caused mainly contains acute poisoning and slow poisoning, can cause pneumonia when acute poisoning is serious; Slow poisoning can cause dermatitis, acne etc. and neurasthenia syndrome etc.The GB2760-1996 food additives use hygienic standard that its usable range is clearly defined, and can not directly add in the food to eat, so the pollution detection of edible oil and fat mineral oil in fluid is a crucial test item.But be based on the dispersiveness of present edible oil and fat production and selling, finish effective monitoring, just need carry out fast measuring a large amount of on-the-spot samples.Mix the detection that (mixing) gone into mineral oil for edible animal and plant grease, mainly contain following method at present both at home and abroad: (1) empirical method, generally adopt sense organ to differentiate, differentiate as smell; (2) physics method is as fluorescence reaction method etc.; (3) chemical method is as saponification method etc.(4) chromatography is as thin-layered chromatography, gas chromatography-mass spectrography etc.Arrived twentieth century beginning of the nineties at the end of the eighties, the microwave catalysis technical development is got up, thereby has produced the microwave saponification method.There were some researchers to test the ultrasound wave saponification method in recent years again.At present, though gas chromatography-mass spectrography, microwave saponification method, ultrasound wave saponification method aspect the qualitative and quantitative analysis of grease mineral oil in fluid accuracy than other quilitative method accuracy height, but since these method complicated operations, the expense height, and their popularization degree is restricted.
And at present the laboratory detection method that is widely used in whether being mixed with in the edible oil and fat mineral oil is saponification method and fluorescence method.But cost of equipment height, the testing result of fluorescence method are extremely undesirable; And the saponification method operating process is comparatively numerous and diverse, and detection time is longer, can't satisfy the needs of on-the-spot supervision and management are sold, transported to edible oil and fat.
Along with government and consumer more and more pay attention to food security, the method for quick of research edible oil and fat mineral oil in fluid seems necessary and urgent.
Summary of the invention
That purpose of the present invention is specialized in out at existing problem in the above-mentioned prior art just is a kind of easy and simple to handle, with low cost, differentiate accurately, the method for quick of low content mineral oil in the edible oil and fat of good reproducibility.
The objective of the invention is to realize by following scheme:
The method for quick of low content mineral oil may further comprise the steps in the edible oil and fat of the present invention: (1) gets oil sample 0.1～2ml to be measured, and the strong base solution that adds isopyknic its concentration and be more than 60% mixes in container; (2) add the ethanol more than 95% of 20～40 times of amounts of this mixed solution then, (3) are inserted this container in 80 ℃～100 ℃ hot baths and are added thermal oscillation 5～30min; (4) add boiling water 15～35ml, occur muddy for containing the judgement of mineral oil to estimate this solution.
Strong base solution described in the present invention can be independent KOH solution or NaOH solution, also can be the two mixed solution, and when being the mixed solution of KOH and NaOH, the volume ratio of its two kinds of solution can be from 2: 1 to 1: 2.
The characteristics of this detection method are without the saponification backflow, by changing the addition of sample and reagent, to adopt and directly carry out saponification in hot bath.
The advantage that the present invention is possessed compared to existing technology is: test apparatus is simple, with low cost; Easy and simple to handle, do not need reflux course; Sample differentiates accurately good reproducibility is easy to judge exactly whether be mixed with mineral oil in the oil, can be used for the production scene of edible oil and fat easily and sell on-the-spot supervision and management, is particularly suitable for basic unit and uses.So this method has overcome to waste time and energy etc. not enoughly when using traditional experimental technique that mineral oil is detected, have a good application prospect.Utilize method of the present invention can work up the quantitative sample of low content mineral oil nephelometry in the edible oil:
Attached: the concrete steps of low content mineral oil nephelometry detection by quantitative in the edible oil:
1. detect the grade of edible oil according to desire, select the edible oil of ad eundem, making the series of standards oil sample of variable concentrations mineral oil---mineral oil content (m/m) is respectively 0,0.1%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0% (significant figure are accurate to 2 significant digits).
2. obtain emulsion according to described step in above-mentioned (1)-(4) and conditional operation, wherein oil sample and highly basic all need accurate weighing (g) in (1) step.Under the 580nm wavelength, survey the light absorption value of emulsion as reference with the oil sample that does not contain mineral oil.
3. the drafting of typical curve: the concentration of mineral oil multiply by the quality that sampling amount promptly is a mineral oil, is horizontal ordinate with the quality of mineral oil, is that ordinate is figure with the light absorption value, draws the typical curve of light absorption value and mineral oil relationship between quality.
4. 2.～3., (m g), as reference, measures the light absorption value of unknown oil sample with the oil sample that do not contain mineral oil to get unknown oil sample as step.According to the light absorption value of unknown sample, obtain the quality (m of corresponding sample mineral oil in fluid by typical curve
1, g), then divided by sample weighting amount, promptly be the mineral oil content of (mainly referring to paraffin) (c, %).
c(％)＝100×m
1/m
Embodiment
The present invention is described further below in conjunction with embodiment, but does not limit the present invention.
Embodiment 1
(1) preparation strong base solution: 60%KOH solution (m/m) and 60%NaOH solution (m/m) are made into mixed solution by 1: 1 volume ratio; (2) oil sample to be measured of adding 1.5ml in the triangular flask (also can select other container) of cleaning adds isopyknic strong base solution and 50ml95% ethanol again; (3) in 100 ℃ boiling water bath, add thermal oscillation 10min; (4) add boiling water 30ml, observe phenomena.
By range estimation as can be known, the oil sample appearance muddiness that contains mineral oil.
If do not contain mineral oil, then muddiness can not appear.
Embodiment 2
(1) preparation strong base solution: 60%NaOH solution (m/m); (2) in the triangular flask of cleaning, add the oil sample of 0.1ml, add the absolute ethyl alcohol of isopyknic strong base solution and 20ml again; (3) in 80 ℃ hot bath, add the about 30min of thermal oscillation; (4) add boiling water 15ml, observe phenomena; (5) absorbance of liquid behind the employing nephelometry mensuration adding boiling water.
Promptly can accurately judge the existence and the content of mineral oil by nephelometry quantitative criterion sample.
Embodiment 3
(1) preparation strong base solution: 60%KOH solution (m/m); (2) in the triangular flask of cleaning, add oil sample about 0.5ml, add 95% ethanol of isopyknic strong base solution and 30ml again; (3) in 85 ℃ hot bath, add thermal oscillation 5min; (4) add boiling water 20ml, observe phenomena;
By range estimation as can be known, the oil sample appearance muddiness that contains mineral oil.
Embodiment 4
(1) preparation strong base solution: 60%KOH solution (m/m) and 60%NaOH solution (m/m) are made into mixed solution by 1: 2 volume ratio; (2) oil sample of adding 1ml in the triangular flask of cleaning adds isopyknic strong base solution and 60ml 95% ethanol again; (3) in 90 ℃ hot bath, add thermal oscillation 20min; (4) add boiling water 30ml, observe phenomena.
By range estimation as can be known, the oil sample appearance muddiness that contains mineral oil.
Embodiment 5
(1) preparation strong base solution: 60%KOH solution (m/m) and 60%NaOH solution (m/m) are made into mixed solution by 2: 1 volume ratio; (2) in the triangular flask of cleaning, add oil sample about 2ml, add 95% ethanol of isopyknic strong base solution and 40ml again; (3) in 95 ℃ hot bath, add thermal oscillation 15min; (4) add boiling water 25ml, observe phenomena.
By range estimation as can be known, the oil sample appearance muddiness that contains mineral oil.
In the various embodiments described above, the detection of edible oil and fat is shown: for the edible oil and fat that mix mineral oil, can use method that the present invention introduces in the extremely short time, need not use valuable experimental apparatus, can determine the existence of its mineral oil in fluid; And its detection limit reaches 0.1% on the basis of nephelometry, exceeds the lowest detectable limit (0.5%) of traditional quilitative method; As solvent, enlarged the scope of experiment reagent with 95% ethanol, absolute ethyl alcohol.More outstanding is, is aided with nephelometry and can reaches quantitative test to the edible oil and fat mineral oil in fluid.
Claims (3)
1, the method for quick of low content mineral oil in a kind of edible oil and fat, it is characterized in that: this detection method may further comprise the steps: (1) gets oil sample 0.1～2ml to be measured, and the strong base solution that adds isopyknic its concentration and be more than 60% mixes in container; (2) add the ethanol more than 95% of 20～40 times of amounts of mixed solution in the step (1) then, (3) are inserted this container in 80 ℃～100 ℃ hot baths and are added thermal oscillation 5～30min; (4) add boiling water 15～35ml, occur muddy with the solution in the range estimation container for containing the judgement of mineral oil.
2, the method for quick of low content mineral oil in the edible oil and fat according to claim 1 is characterized in that: strong base solution is KOH solution, NaOH solution or the two mixed solution.
3, the method for quick of low content mineral oil in the edible oil and fat according to claim 2 is characterized in that: when strong base solution was the mixed solution of KOH and NaOH, the volume ratio of its two kinds of solution was 2: 1～1: 2.
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| CN100437094C true CN100437094C (en) | 2008-11-26 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101893577A (en) * | 2010-06-21 | 2010-11-24 | 罗付生 | Quick identification method of discolored hogwash oil (swill-cooked dirty oil) |
| CN103743857A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Croton oil detection reagent and application thereof |
| CN103743741A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Mineral oil detection reagent and application thereof |
| CN103743860A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Tung oil detection reagent and application thereof |
| CN106468664B (en) * | 2015-08-14 | 2019-06-14 | 中国石油化工股份有限公司 | A kind of detection method of fast qualitative barium strontium ion |
| CN112051224B (en) * | 2020-08-12 | 2021-08-06 | 昆明理工大学 | Method for detecting blending ratio of biodiesel blending fuel based on ultraviolet-visible spectrophotometry |
Citations (1)
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|---|---|---|---|---|
| CN1654946A (en) * | 2004-02-12 | 2005-08-17 | 陈平 | Quick test method for mineral oil in food |
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| CN1654946A (en) * | 2004-02-12 | 2005-08-17 | 陈平 | Quick test method for mineral oil in food |
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Assignee: Shenzhen Pony Test Technology Co., Ltd. Assignor: Henan Industry University Contract fulfillment period: 2008.12.20 to 2013.12.19 contract change Contract record no.: 2009990000190 Denomination of invention: Method for fast detecting low-content mineral oil in edible oil and fat Granted publication date: 20081126 License type: Exclusive license Record date: 2009.3.17 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.12.20 TO 2013.12.19; CHANGE OF CONTRACT Name of requester: SHENZHEN CITY PUNI TEST TECHNOLOGY CO., LTD. Effective date: 20090317 |
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