CN101846611B - Method for determining oil content of vegetable oil material based on ultrasonic assistant extraction - Google Patents
Method for determining oil content of vegetable oil material based on ultrasonic assistant extraction Download PDFInfo
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- CN101846611B CN101846611B CN2010101903750A CN201010190375A CN101846611B CN 101846611 B CN101846611 B CN 101846611B CN 2010101903750 A CN2010101903750 A CN 2010101903750A CN 201010190375 A CN201010190375 A CN 201010190375A CN 101846611 B CN101846611 B CN 101846611B
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Abstract
The invention discloses a method for determining oil content of vegetable oil material. The method utilizes an ultrasonic wave as an assistant tool, and comprises the steps of sampling, sample preparation, solvent ultrasonic assistant extraction, solvent recovery, extract drying, oil content calculation and the like. The method can completely and quickly extract and determine crude fat in the vegetable oil material, and can greatly speed up the process of extracting the crude fat in the oil material so as to shorten the determination time of the vegetable oil material. Compared with the conventional Soxhlet extraction method, the method has the advantages of simple operation, short consumed time, accurate determination result, good repeatability and the like, and is a novel method for quickly determining the oil content of the vegetable oil material.
Description
Technical field
The invention belongs to the chemical analysis detection range, be specifically related to a kind of assay method of oil content of vegetable oil material.
Background technology
Oil content of vegetable oil material is an important chemical constitution, is to be used for one of important indicator of evaluating oil plant quality and nutritive value, and for oil plant, the height of oleaginousness directly shows the economic worth of oil plant; Simultaneously, the height of oleaginousness also is an important evidence of determining the oil plant grade.
At present, the national standard method of inspection of measuring at China's oil content of vegetable oil material is the Soxhlet extraction process, comprises GB/T5512-2008, GB/T6433-2006, GB/T14488.1-2008 etc.The Soxhlet extraction process is to utilize ether or sherwood oil as solvent, uses the Soxhlet extraction plant, ether in the vegetable oil material or petroleum ether soluble matter are extracted, and removes and desolvates, and the quality of weighing extract is calculated oleaginousness.Though crude fat can be reclaimed by the extracting bottle fully in this method sample, measurement result accurately and reliably, but test period length, dangerous height, whole experiment are finished probably needs (only the extracting time just needs 6-8 hour to wherein individual sample) about 10-12 hour, consume a large amount of water power etc., is difficult to satisfy the real work needs sometimes.
Chinese scholars is improved the Soxhlet extraction process, has developed new detection method, as fat test instrument method, Abbe refractometer method, nuclear magnetic resonance method, near-infrared absorption spectrum method etc.When fat test instrument method is measured oil content in plants, extraction temperature, boiling extracting time, drip washing time and extract solvent and the sample granularity all has bigger influence to measurement result, and need to consume a certain amount of water power, experiment danger is bigger; Abbe refractometer method, nuclear magnetic resonance method, near-infrared absorption spectrum are owned by France in indirect assay method, and its measurement result is a benchmark with the Soxhlet extraction process all, and the price of nuclear magnetic resonance analyser and near infrared spectrometer is comparatively expensive, has limited it and has applied.Therefore, seek a kind of easy and simple to handle, result accurately, the oil content of vegetable oil material assay method of favorable reproducibility, be that those skilled in the art pay close attention to always.
Summary of the invention
Defective or deficiency at above-mentioned prior art existence, the objective of the invention is to, a kind of method based on the auxiliary lixiviate mensuration of ultrasound wave oil content of vegetable oil material is provided, this method utilizes ultrasound wave as aid, can extract in the vegetable oil material crude fat fully and measured, can quicken the leaching process of crude fat in the oil plant greatly, thereby shorten the vegetable oil material minute.
In order to realize above-mentioned task, the technical scheme that the present invention takes is:
A kind of method based on the auxiliary lixiviate mensuration of ultrasound wave oil content of vegetable oil material is characterized in that, comprises the following steps:
1) sampling: get vegetable oil material sample to be measured, described vegetable oil material sample to be measured does not contain other impurity and breakage and rotten oil plant in storage and transportation;
2) specimen preparation: take by weighing sample 5.0g～10.0g with the baking box, and the sample that takes by weighing is accurate to 0.001g, place 105 ℃ baking oven to dry 30min, pour into while hot in the mortar, add 4g degreasing fine sand, together grind, sample and fine sand are ground after go out oily harmless changing in the triangular flask;
3) the auxiliary lixiviate of ultrasound wave: in triangular flask, add sherwood oil, the ratio of sample and sherwood oil is 1:12W/V～1:20W/V, in ultrasonic frequency is that 45KHz～100KHz, ultrasonic power are lixiviate 10-15min under the condition of 90W～100W, collect leaching liquor, lixiviate is 4 times～6 times repeatedly, merges leaching liquor;
4) the heating leaching liquor reclaims sherwood oil, and the extract that obtains, places 105 ℃ of baking ovens, behind the baking 90min, dries 30min more earlier, dry by the fire to extract and reach constant weight, promptly before and after the difference of twice weighing result be constant weight less than 5mg;
5) calculating of oil content of vegetable oil material to be measured is undertaken by following formula:
W=m
2/ m
1* 100%; In the formula, w is an oil content of vegetable oil material to be measured, m
1Be the quality of sample, g; m
2Be the quality of constant weight extract, g; Can obtain the oleaginousness of vegetable oil material to be measured.
Method of the present invention is easy and simple to handle, the result accurate, favorable reproducibility, provides a kind of new method for measuring oil content of vegetable oil material, and this method not only can be used as the vegetable oil material assay, also can be used for the food crude fat content simultaneously and measure.
Application the present invention is based on the method that oil content of vegetable oil material is measured in the auxiliary lixiviate of ultrasound wave, and the technique effect that brings is as follows:
(1) based on the auxiliary lixiviate of ultrasound wave, can shorten the time that vegetable oil material crude fat is measured greatly, the national standard method minute can be foreshortened to 3-4 hour in 10-12 hour.
(2) method to the instrument of measuring require simple, easy and simple to handle, need not a large amount of chilled waters, can be used as the alternative method that national standard is measured the vegetable oil material crude fat content, it has a extensive future.
Embodiment
The present invention is described in further detail below in conjunction with embodiment that the inventor provides.
Ultrasound wave is the sound wave of a kind of vibration frequency more than 20KHz, and ultrasonic technique is applied to extract the existing report of researchs such as lipid in the plant, alkaloid, glycoside, bioactivator.This technology has the advantages that energy consumption is low, efficient is high, do not destroy effective constituent.Much studies show that, utilize judder that ultrasound wave produces, high acceleration, strong cavitation effect, beating action etc., the effective constituent that can quicken in the plant enters solvent, thereby raising extraction ratio of effective constituents, shorten extraction time, and can avoid high temperature extracting the influence of composition.
In order to determine the auxiliary extracting technology of ultrasound wave, the applicant has carried out experiment to the auxiliary lixiviate optimum process condition of ultrasound wave and has determined, experiment is a raw material with yellow mustard seed oil, ultrasonic technique is optimized, at first on the basis of experiment of single factor, choosing solid-liquid ratio, ultrasonic frequency, ultrasonic power and extraction time is empirical factor, is test index with the oil yield, three hydraulic tests of four factors are set, and select L for use
27(3
13) orthogonal arrage arrangement test, each test combinations repeats twice, averages.
The method of concrete experiment comprises:
(1) yellow mustard seed picks up from the Yulin, natural air drying, removal of impurities, uniform sampling.
(2) yellow mustard seed specimen preparation: take by weighing a certain amount of sample with the baking box, sample is accurate to 0.001g, places 105 ℃ baking oven to dry 30min, pour into while hot in the mortar, add about 4g degreasing fine sand, together grind, sample and fine sand are ground after go out oily harmless changing in the tool plug triangular flask.
(3) single factor experiment condition setting (extracting temperature all at room temperature carries out);
1) solid-liquid ratio is to the influence of oil yield: ultrasonic frequency is that 45KHZ, ultrasonic power are that 80W, extraction time are 10min, solid-liquid ratio (w/v) is set is 1:4,1:6,1:8,1:10,1:12,1:14,1:16,1:20, the research solid-liquid ratio is to the influence of oil yield.
2) influence of ultrasonic frequency comparison oil yield: solid-liquid ratio is 1:12(w/v), ultrasonic power is that 80W, extraction time are 10min, ultrasonic frequency is set for being 45KHZ, 80KHZ, 100KHZ, the research ultrasonic frequency is to the influence of oil yield.
3) ultrasonic power is to the influence of oil yield: ultrasonic frequency is that 45KHZ, solid-liquid ratio are 1:12(w/v), extraction time is 10min, it is 20W, 40W, 60W, 80W, 100W that ultrasonic power is set, the research ultrasonic power is to the influence of oil yield.
4) extraction time is to the influence of oil yield: ultrasonic frequency is that 45KHZ, solid-liquid ratio are 1:12(w/v), ultrasonic power is 80W, it is 5min, 10min, 15min, 20min, 35min that extraction time is set, and research surpasses the influence of extraction time to oil yield.
(4) on the single factor analysis basis, choose ultrasonic frequency (45KHZ, 80KHZ, 100KHZ), ultrasonic power (80W, 90W, 100W), solid-liquid ratio (w/v) (1:10,1:12,1:14), extraction time, (10min, 20min, 30min) carried out orthogonal test.
By the Orthogonal experiment results analysis, the optimum worker's condition that draws is: solid-liquid ratio is 1:12(W/V), be that 45KHz, ultrasonic power are that 90W, extraction time are 10min in ultrasonic frequency, yellow mustard seed oil yield is that the yellow mustard seed of 30.9%(oleaginousness is 31.3%), the oil extracting rate under the optimum process can reach 98.7%.
The present invention utilizes the characteristic of ultrasound wave rapid extraction to extract fat content in the vegetable oil material, by condition optimizing frequency of ultrasonic and power, extraction time, solid-liquid ratio etc., under optimal conditions, extract crude fat in the vegetable oil material, and the oleaginousness of vegetable oil material is carried out determination and analysis.
It below is the specific embodiment that the inventor provides, need to prove that following examples have provided the mensuration of the vegetable oil material of high, medium and low oleaginousness respectively, the invention is not restricted to these embodiment, according to method of the present invention, all can realize oleaginousness mensuration to any vegetable oil material.
Embodiment 1: yellow mustard seed oleaginousness is measured
(1) yellow mustard seed picks up from the Yulin, natural air drying, removal of impurities, uniform sampling.
(2) yellow mustard seed specimen preparation: take by weighing 5.0g-10.0g sample (m with the baking box
1), sample is accurate to 0.001g, places 105 ℃ baking oven to dry 30min, pours into while hot in the mortar, adds about 4g degreasing fine sand, together grinds, and sample and fine sand is ground after go out oily harmless changing in the tool plug triangular flask.
(3) the auxiliary lixiviate of ultrasound wave: according to sample and sherwood oil solid-liquid ratio (sample weight and sherwood oil volume ratio) is 1:12(w/v) the adding sherwood oil.Triangular flask is placed ultrasonoscope, and setting ultrasonic frequency is that 45KHz, ultrasonic power are under the condition of 90W, and lixiviate 15min collects leaching liquor by the mode of suction filtration; Lixiviate is 4 times so repeatedly, merges leaching liquor.
(4) leaching liquor reclaims sherwood oil to collecting leaching liquor in Rotary Evaporators, and the extract that obtains places 105 ℃ of baking ovens, behind the baking 90min, dries by the fire 30min. again to extract constant weight (m earlier
2), promptly the difference of twice weighing result in front and back is less than 5mg.
(5) yellow mustard seed oil oleaginousness (w) computing formula is: w=m
2/ m
1* 100%, do three parallel laboratory tests, in the formula, m
1Be sample, m
2Be the constant weight extract.
(6) in strict accordance with GB/T5512-2008, measure the oleaginousness of yellow mustard seed with the Soxhlet extraction process, also do three parallel laboratory tests.
The measurement result comparative analysis sees Table 1:
Table 1: yellow mustard seed oleaginousness measurement result comparison (%, w/w)
As can be seen from Table 1, the mean value of the auxiliary extraction of supercritical ultrasonics technology of the present invention and Soxhlet extraction process mensuration be respectively 31.2% and 31.3%, two kind of method measurement result deviation be 0.1%, do not have the significance difference opposite sex.From extraction time, in the national standard method extraction time be 8 hours be to compare in 1 hour with the supercritical ultrasonics technology extraction time, shortened 7 hours.This shows that it is fully feasible that the auxiliary extraction of ultrasound wave is measured yellow mustard seed oleaginousness, and measure the required time and shorten greatly.
Embodiment 2: the tea seed oleaginousness is measured
(1) tea seed picks up from the Fujian Youxi, and natural air drying, shells at removal of impurities, evenly gets camellia seed kernel.
(2) camellia seed kernel specimen preparation: take by weighing 5.0g-10.0g sample (m with the baking box
1), sample (m
1) be accurate to 0.001g, place 105 ℃ baking oven to dry 30min, pour into while hot in the mortar, add about 4g degreasing fine sand, together grind, sample and fine sand are ground after go out oily harmless changing in the tool plug triangular flask.
(3) the auxiliary lixiviate of ultrasound wave: according to sample and sherwood oil solid-liquid ratio (weight and volume ratio) is 1:13(w/v) the adding sherwood oil.Tool plug triangular flask is placed ultrasonic washing instrument, and the setting ultrasonic frequency is that 45KHz, ultrasonic power are lixiviate 12min under the condition of 90W, collects leaching liquor by the centrifuging mode; Lixiviate is 5 times so repeatedly, merges leaching liquor.
(4) reclaim sherwood oil in the leaching liquor Rotary Evaporators, the extract that obtains places 105 ℃ of baking ovens, behind the oven dry 90min, behind the baking 90min, dries by the fire 30min. again to extract constant weight (m earlier
2), promptly the difference of twice weighing result in front and back is less than 5mg.
(5) camellia seed oil oleaginousness (w) computing formula is; W=m
2/ m
1* 100%; Do three parallel laboratory tests, in the formula, m
1Be sample, m
2Be the constant weight extract.
(6),, three parallel laboratory tests have also been done with the oleaginousness of Soxhlet extracting mensuration oil tea in strict accordance with GB/T5512-2008.
The measurement result comparative analysis sees Table 2.
Table 2: tea seed oleaginousness measurement result relatively
As can be seen from Table 2, the mean value of the auxiliary extraction of supercritical ultrasonics technology of the present invention and Soxhlet extraction process mensuration be respectively 55.8% and 55.6%, two kind of method measurement result deviation be 0.2%, do not have the significance difference opposite sex.In addition, be single factor with different measuring methods, carry out the experiment of single factor analysis, show between the auxiliary extraction of supercritical ultrasonics technology and two kinds of methods of Soxhlet extraction process difference not remarkable (P＜0.01).From extraction time, the extraction time of national standard method be 8 hours be to compare in 1 hour with the supercritical ultrasonics technology extraction time, shortened 7 hours.This shows that it is fully feasible that the auxiliary extraction of ultrasound wave is measured the tea seed oleaginousness, and measure the required time and shorten greatly.
Should be noted in the discussion above that if twice weighing weightening finish surpasses 5mg before and after the extract in the foregoing description 1,2, think that then extract is oxidized in dry run, should change drying condition, under 80 ℃ of vacuum conditions, carry out, prevent Oxidation of Fat and Oils.
Embodiment 3: the walnut kernel oleaginousness is measured
(1) walnut picks up from Shaanxi Huanglong, and walnut kernel is peeled off, evenly got to natural air drying, at removal of impurities.
(2) walnut kernel specimen preparation:, take by weighing 5.0g-10.0g sample (m with the baking box with the walnut kernel section
1), sample (m
1) be accurate to 0.001g, place 105 ℃ baking oven to dry 30min, pour into while hot in the mortar, add about 4g degreasing fine sand, together grind, sample and fine sand are ground after go out oily harmless changing in the tool plug triangular flask.
(3) the auxiliary lixiviate of ultrasound wave: pressing sample and sherwood oil solid-liquid ratio (weight and volume ratio) is 1:14(w/v) the adding sherwood oil.Tool plug triangular flask is placed ultrasonic washing instrument, and the setting ultrasonic frequency is that 45KHz, ultrasonic power are lixiviate 10min under the condition of 100W, collects leaching liquor by the mode that filters; Extracting is 6 times so repeatedly, merges leaching liquor.
(4) leaching liquor reclaims sherwood oil in Rotary Evaporators, obtains extract, and extract is placed 80 ℃ of vacuum drying ovens (vacuum tightness is 0.1MPa), behind the baking 90min, dries by the fire 30min. again to extract constant weight (m earlier
2) (difference of twice weighing result in front and back is less than 5mg).
(5) walnut kernel oleaginousness (w) computing formula is w=m
2/ m
1* 100%, do three parallel laboratory tests, in the formula, m
1Be sample, m
2Be the constant weight extract.
(6) in strict accordance with the oleaginousness of GB/T5512-2008, also do three parallel laboratory tests with Soxhlet extracting mensuration walnut kernel.
The measurement result comparative analysis sees Table 3.
Table 3: walnut kernel oleaginousness measurement result relatively
As can be seen from Table 3, the mean value of the auxiliary extraction of supercritical ultrasonics technology and Soxhlet extraction process mensuration be respectively 66.2% and 66.4%, two kind of method measurement result deviation be 0.2%, do not have the significance difference opposite sex.In addition, be single factor with different measuring methods, carry out the experiment of single factor analysis, show between the auxiliary extraction of supercritical ultrasonics technology and two kinds of methods of Soxhlet extraction process difference not remarkable (P＜0.01).From extraction time, the extraction time of national standard method be 8 hours be to compare in 1 hour with the supercritical ultrasonics technology extraction time, shortened 7 hours.This shows that it is fully feasible that the auxiliary extraction of ultrasound wave is measured the walnut kernel oleaginousness, and measure the required time and shorten greatly.
More than by three kinds of specific embodiments, having chosen three kinds of vegetable oil materials that belong to high, medium and low oleaginousness respectively is analyzed, as can be seen, its result of vegetable oil material that ultrasound wave assisted extraction method of the present invention is measured different oleaginousness compares there was no significant difference with traditional Soxhlet extraction process, the oleaginousness that ultrasound wave assisted extraction method mensuration vegetable oil material of the present invention is described is feasible fully, and can shorten the needed time of measuring greatly, need not a large amount of chilled waters, is the new method that a kind of oil content of vegetable oil material is measured.
Claims (1)
1. the method based on the auxiliary lixiviate mensuration of ultrasound wave oil content of vegetable oil material is characterized in that, comprises the following steps:
1) sampling: get vegetable oil material sample to be measured, described vegetable oil material sample to be measured does not contain other impurity and breakage and rotten oil plant in storage and transportation;
2) specimen preparation: take by weighing sample 5.0g～10.0g with the baking box, and the sample that takes by weighing is accurate to 0.001g, place 105 ℃ baking oven to dry 30min, pour into while hot in the mortar, add 4g degreasing fine sand, together grind, sample and fine sand are ground after go out oily harmless changing in the triangular flask;
3) the auxiliary lixiviate of ultrasound wave: in triangular flask, add sherwood oil, the solid-liquid ratio of sample and sherwood oil is 1:12 W/V～1:20W/V, in ultrasonic frequency is that 45KHz～100KHz, ultrasonic power are lixiviate 10min～15min under the condition of 90W～100W, collect leaching liquor, lixiviate is 4 times～6 times repeatedly, merges leaching liquor;
4) the heating leaching liquor reclaims sherwood oil, and the extract that obtains, places 105 ℃ of baking ovens, earlier behind the baking 90min, dry 30min again, reach constant weight if dry by the fire to extract, the difference of twice weighing result is a constant weight less than 5mg promptly, and then execution in step 5), otherwise execution in step 4 ');
4 ') carry out following steps execution in step 1 once more)-3):
The heating leaching liquor reclaims sherwood oil, and the extract that obtains, places 80 ℃ of vacuum drying ovens, behind the baking 90min, dries 30min more earlier, dry by the fire to extract and reach constant weight, promptly before and after the difference of twice weighing result be constant weight less than 5mg; Afterwards, execution in step 5);
5) be calculated as follows and obtain oil content of vegetable oil material to be measured:
w=m
2/m
1×100%；
In the formula, w is an oil content of vegetable oil material to be measured, m
1Be the quality of sample, mass unit: gram; m
2Be the quality of constant weight extract, mass unit: gram.
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| CN103278420A (en) * | 2013-05-24 | 2013-09-04 | 西南大学 | Method for rapidly measuring content of crude fat in food |
| CN104181080B (en) * | 2014-08-28 | 2016-08-24 | 湖南中科富邦科技有限责任公司 | A kind of sump oil water oil-containing method of real-time and monitoring device thereof |
| CN106053281A (en) * | 2016-06-21 | 2016-10-26 | 中国热带农业科学院香料饮料研究所 | Method for detecting content of fat in Piper plant |
| CN108169058A (en) * | 2017-12-19 | 2018-06-15 | 天邦食品股份有限公司 | A kind of method of crude fat content in rapid and accurate determination feed |
| CN111307644A (en) * | 2019-12-02 | 2020-06-19 | 江苏厚生新能源科技有限公司 | Method for measuring oil content of high-strength thinned polyolefin porous membrane |
| CN114486606A (en) * | 2020-11-13 | 2022-05-13 | 中国石油天然气股份有限公司 | Method for measuring oil content |
| CN114923804A (en) * | 2022-03-09 | 2022-08-19 | 陇南市祥宇油橄榄开发有限责任公司 | Method for determining fat content in olive fruit |
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