CN103278420A - Method for rapidly measuring content of crude fat in food - Google Patents
Method for rapidly measuring content of crude fat in food Download PDFInfo
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- CN103278420A CN103278420A CN2013101973189A CN201310197318A CN103278420A CN 103278420 A CN103278420 A CN 103278420A CN 2013101973189 A CN2013101973189 A CN 2013101973189A CN 201310197318 A CN201310197318 A CN 201310197318A CN 103278420 A CN103278420 A CN 103278420A
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Abstract
The invention relates to a method for rapidly measuring the content of crude fat in food. The method comprises the steps of extracting the crude fat from food by treating a sample, weighing, adding petroleum ether into the sample, carrying out ultrasonic extraction and the like and with an ultrasonic technology, and calculating the content of the crude fat of the sample according to the mass difference before and after the crude fat of the food sample is extracted. Compared with the prior art, the method not only shortens the crude fat measurement time to 50min-150min from 8h-12h, but also can be used for measuring a plurality of or even dozens of samples at the same time for once according to the size of an ultrasonic cleaner.
Description
Technical field
The present invention relates to the Food Inspection technical field, particularly relate to the method for crude fat content in a kind of quick mensuration food.
Background technology
Lipid in the food mainly comprises fat (triglyceride) and some lipid materials, as fatty acid, phosphatide, glycolipid, sterol, sterol etc.The method of measuring lipid commonly used have soxhlet extraction, acid-ether method, Luo Zi – Gothic in method etc.Soxhlet extraction is to measure classics, the representational method that lipid material (crude fat) content generally adopts in the food, also is one of assay method of national Specification.But this method is time-consuming, measure a sample and generally need reach 8～12h, and the consumption of solvent is also bigger.Up to the present, still there is not the relevant research report of measuring crude fat content method in the food fast.
Summary of the invention
Problem in view of the prior art existence, the object of the present invention is to provide the method for crude fat content in a kind of quick mensuration food, the inventive method is utilized ultrasonic technology, crude fat is proposed from food, be suggested the of poor quality of front and back, the crude fat content of calculation sample according to food samples crude fat.
Ultrasound wave refers to that frequency is the mechanical wave about 20 kilo hertzs～50 megahertzes, and it has multistage physical influences such as cavitation, the higher-order of oscillation and microjet, can accelerate the stripping of fat.
The method of crude fat content in a kind of quick mensuration food of the present invention, realize successively through the following steps:
(1) get food samples to be measured, the baking oven of putting into 95～105 ℃ after the pulverizing is dried to constant weight, gets the fresh and dried f of ratio with the quality before dry divided by dried quality;
(2) take by weighing the food samples quality m1 to be measured that is dried to constant weight, wrap into the quantitative filter paper (the about 9cm of diameter) that in 70 ℃ of baking ovens, is dried to constant weight quality m2;
(3) filter paper packet that will be surrounded by food samples to be measured is put into glass container, add sherwood oil, the mass volume ratio of food samples to be measured and sherwood oil is 1g:15～80mL in the filter paper packet, glass container is put into supersonic wave cleaning machine, be 50～150w at power, temperature is 30 ℃ of ultrasonic extraction 15～50min down, and sherwood oil is poured out, and same operation repeats to extract 3 times;
(4) filter paper packet is taken out, in 70 ℃ baking oven, be dried to constant weight quality m3, according to the crude fat content in the following formula calculation sample:
The crude fat content of sample (%)=
The inventive method is used for the fair 1g that is no more than of the food samples to be measured of ultrasonic extraction.
Advantage of the present invention is:
Compared with prior art, the time that the inventive method not only will be measured crude fat has shortened to 50～150min from 8～12h, and according to the size of supersonic wave cleaning machine, once can measure several and even dozens of sample simultaneously.
Embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, below the preferred embodiments of the present invention is described in detail.
The mensuration of crude fat content in embodiment 1 silkworm chrysalis
Silkworm chrysalis contains abundant fat.The silkworm chrysalis sample can be directly used in the mensuration of crude fat through dry.
(1) the silkworm chrysalis sample is pulverized, put into the polybag sealing and preserve standby;
(2) cut-off is directly put into 70 ℃ of baking ovens for 6 of the quantitative filter papers of 9cm and is dried to constant weight, preserves standby in exsiccator;
(3) get one of the filter paper that is dried to constant weight, weigh recording quality (g);
(4) take by weighing the silkworm chrysalis sample of pulverizing at filter paper, recording quality (g);
With filter paper dried silkworm chrysalis meal is wrapped, attention can not spill.
(5) filter paper packet that will be surrounded by sample is put into blue cover glass bottle, adds the sherwood oil of 60～90 ℃ of 20mL, boiling range in the bottle, builds bottle cap, and blue cover glass bottle is put into supersonic wave cleaning machine.Ultrasonic power is decided to be 60w, and temperature is 30 ℃, behind the ultrasonic extraction 50min, the sherwood oil in the bottle is poured out; Add the 20mL sherwood oil again in bottle, ultrasonic extraction 50min so repeats to extract 3 times;
The sherwood oil of pouring out can reclaim, re-use after the redistillation.
(6) will take out through the filter paper packet after the ultrasonic processing, in 70 ℃ of baking ovens, filter paper packet will be dried to constant weight, weighing, recording quality (g).The quality that reduce the ultrasonic back of filter paper packet is the quality of crude fat in the sample.
(7) 6 results of crude fat content replication such as following table (%) in the silkworm chrysalis
| Numbering | Filter paper (g) | Sample (g) | Ultrasonic and dry back filter paper packet quality (g) | Crude fat content (%) | Mean+SD |
| 1 | 0.745 | 0.505 | 1.083 | 33.069 | 32.736±1.010 |
| 2 | 0.750 | 0.485 | 1.084 | 31.134 | ? |
| 3 | 0.752 | 0.475 | 1.072 | 32.632 | ? |
| 4 | 0.736 | 0.461 | 1.039 | 34.273 | ? |
| 5 | 0.745 | 0.332 | 0.969 | 32.530 | ? |
| 6 | 0.745 | 0.479 | 1.067 | 32.777 | ? |
By measurement result as can be known, the mean value with crude fat content in the inventive method mensuration silkworm chrysalis is 32.74%.
Measure crude fat content (%) in the same silkworm chrysalis sample with soxhlet extraction, the result is as follows:
| ? | ? | Before the extracting | ? | After the extracting | ? | ? |
| Numbering | Filter paper quality (g) | Sample+paper (g) | Sample quality (g) | Sample+paper (g) | Crude fat quality (g) | Crude fat content (%) |
| 1 | 0.771 | 1.097 | 0.326 | 0.993 | 0.104 | 31.90 |
| 2 | 0.737 | 1.075 | 0.338 | 0.966 | 0.109 | 32.25 |
| 3 | 0.745 | 1.142 | 0.397 | 1.015 | 0.127 | 31.99 |
| 4 | 0.768 | 1.017 | 0.249 | 0.935 | 0.082 | 32.93 |
| 5 | 0.752 | 1.049 | 0.297 | 0.952 | 0.097 | 32.66 |
| 6 | 0.76 | 1.047 | 0.287 | 0.955 | 0.092 | 32.05 |
| 7 | 0.761 | 1.052 | 0.291 | 0.952 | 0.1 | 34.36 |
| Mean value | ? | ? | ? | ? | 0.102 | 32.59 |
| Standard deviation | ? | ? | ? | ? | 0.014 | 0.87 |
By measurement result as can be known, the mean value with crude fat content in the silkworm chrysalis of soxhlet extraction mensuration is 32.59%.
Measurement result shows that the crude fat content difference does not have conspicuousness in the silkworm chrysalis that the soxhlet extraction of the inventive method and classics is measured.
The mensuration of crude fat in the embodiment 2 dried mulberry leaf
(1) processing of filter paper: cut-off is directly put into 70 ℃ of baking ovens for 6 of the quantitative filter papers of 9cm and is dried to constant weight, preserves standby in exsiccator;
(2) get one of the filter paper that is dried to constant weight, weigh recording quality (g);
(3) dried mulberry leaf powder of pulverizing at the filter paper title, recording quality (g);
With filter paper mulberry leaf powder is wrapped, attention can not spill.
(4) filter paper packet that will be surrounded by mulberry leaf powder is put into blue cover glass bottle, add the sherwood oil of 60～90 ℃ of 20mL, boiling range in the bottle, build bottle cap, blue cover glass bottle is put into supersonic wave cleaning machine, ultrasonic power is decided to be 150w, temperature is 30 ℃, behind the ultrasonic 15min, the sherwood oil in the bottle is poured out, add the 20mL sherwood oil again, ultrasonic 15min pours out sherwood oil, so repeats to extract 3 times;
(5) filter paper packet is taken out from bottle, 70 ℃ of oven for drying to constant weight, weighing, recording quality (g).Filter paper packet is the quality of crude fat in the sample through the ultrasonic quality of handling the back minimizing.
(6) 6 dried mulberry leaf crude fat content of replication (%)
| Numbering | Filter paper (g) | Sample (g) | Ultrasonic processing back filter paper packet quality (g) | Crude fat content (%) | Mean+SD |
| 1 | 0.750 | 0.345 | 1.067 | 8.116 | 9.318±0.808 |
| 2 | 0.762 | 0.324 | 1.056 | 9.259 | ? |
| 3 | 0.747 | 0.305 | 1.021 | 10.164 | ? |
| 4 | 0.764 | 0.27 | 1.009 | 9.259 | ? |
| 5 | 0.754 | 0.305 | 1.032 | 8.852 | ? |
| 6 | 0.747 | 0.312 | 1.027 | 10.256 | ? |
By measurement result as can be known, the mean value by crude fat content in the dried mulberry leaf of the inventive method mensuration is 9.32%.
Measure crude fat content (%) in the same dried mulberry leaf sample with soxhlet extraction, the result is as follows:
| ? | ? | Before the extracting | ? | After the extracting | ? | ? |
| Numbering | Filter paper quality (g) | Sample+paper (g) | Sample quality (g) | Sample+paper (g) | Crude fat quality (g) | Crude fat content (%) |
| 1 | 0.752 | 1.031 | 0.279 | 1.002 | 0.029 | 10.394 |
| 2 | 0.758 | 1.084 | 0.326 | 1.051 | 0.033 | 10.123 |
| 3 | 0.743 | 1.084 | 0.341 | 1.051 | 0.033 | 9.677 |
| 4 | 0.747 | 1.061 | 0.314 | 1.033 | 0.028 | 8.917 |
| 5 | 0.747 | 1.054 | 0.307 | 1.025 | 0.029 | 9.446 |
| 6 | 0.751 | 1.031 | 0.28 | 1.005 | 0.026 | 9.286 |
| Mean value | ? | ? | ? | ? | 0.030 | 9.641 |
| Standard deviation | ? | ? | ? | ? | 0.003 | 0.546 |
By measurement result as can be known, the mean value with crude fat content in the dried mulberry leaf of soxhlet extraction mensuration is 9.641%.
Measurement result shows that the crude fat content difference does not have conspicuousness in the dried mulberry leaf that the soxhlet extraction of the inventive method and classics is measured.
The mensuration of crude fat in embodiment 3 fresh mulberry leafs
(1) processing of fresh mulberry leaf: beaker is dried in baking oven to constant weight; With the fresh mulberry leaf chopping, take by weighing 100g and put into the beaker of doing to constant weight, the baking oven of putting into 95 ℃ of temperature then is dried to constant weight, weighs.Calculating the fresh and dried of mulberry leaf sample is 4 than f, i.e. 4g fresh mulberry leaf sample oven dry obtains the dried mulberry leaf sample of 1g.
(2) get one of the filter paper that is dried to constant weight, weigh recording quality (g).
(3) the dried mulberry leaf sample of pulverizing at the filter paper title, recording quality (g).With filter paper the sample of weighing is wrapped, attention can not have sample to spill.
(4) filter paper packet that will be surrounded by sample is put into blue cover glass bottle, adds the sherwood oil of 60～90 ℃ of 20mL, boiling range in the bottle, builds bottle cap; Blue cover glass bottle is put into supersonic wave cleaning machine, ultrasonic power is decided to be 100w, temperature is 30 ℃, behind the ultrasonic 20min, the sherwood oil in the bottle is poured out, added the sherwood oil of 60～90 ℃ of 20mL, boiling range again, pour out sherwood oil behind the ultrasonic 20min, so repeat to extract 3 times.
(5) filter paper packet is taken out, put into 70 ℃ of baking ovens filter paper packet is dried to constant weight, weighing, recording quality (g).
The ultrasonic quality of handling the back minimizing of filter paper packet is the quality of crude fat in the sample.
(7) with crude fat content (%) in the fresh mulberry leaf of the inventive method and soxhlet extraction mensuration:
| Numbering | Filter paper (g) | Sample (g) | Ultrasonic processing back filter paper packet quality (g) | The present invention records crude fat content (%) | The Soxhlet method records crude fat content (%) |
| 1 | 0.766 | 0.991 | 1.657 | 2.523 | 2.543 |
| 2 | 0.779 | 1.012 | 1.696 | 2.347 | 2.312 |
| 3 | 0.775 | 0.912 | 1.594 | 2.549 | 2.611 |
| 4 | 0.773 | 1.082 | 1.736 | 2.749 | 2.307 |
| 5 | 0.768 | 1.144 | 1.775 | 2.994 | 2.195 |
| 6 | 0.780 | 0.964 | 1.665 | 2.049 | 2.433 |
| Mean value ± mark is poor | ? | ? | ? | 2.533±0.325 | 2.400±0.158 |
By measurement result as can be known, the mean value of crude fat content is 2.535% in the fresh mulberry leaf of the inventive method mensuration; What soxhlet extraction was measured is 2.400%, and the two difference does not have conspicuousness.
Attention: when calculating the crude fat content of bright sample, the quality of sample must be converted into fresh weight by dry weight.(be that quality with dried mulberry leaf multiply by 4 quality that namely obtain fresh mulberry leaf in this example.）
The mensuration of crude fat in the embodiment 4 bright capsicums
(1) processing of bright capsicum: beaker is dried to constant weight in baking oven.9 bright capsicum samples are pulverized, taken by weighing 50g respectively in the beaker of constant weight, the baking oven of putting into 100 ℃ then is dried to constant weight, weighs.Calculate the fresh and dried ratio of bright capsicum sample; (2) stand-by filter paper being put into baking oven dries to constant weight.Get one of the filter paper that is dried to constant weight, weigh recording quality (g).
(3) take by weighing about the capsicum sample 0.2g of pulverizing and drying recording quality (g) at filter paper.Wrap with filter paper, attention can not have sample to spill.
(4) filter paper packet that will be surrounded by sample is put into blue cover glass bottle, adds the sherwood oil of 60～90 ℃ of 20mL, boiling range in the bottle, builds bottle cap.Blue cover glass bottle is put into supersonic wave cleaning machine, ultrasonic power is decided to be 100w, temperature is 30 ℃, behind the ultrasonic 40min, the sherwood oil in the bottle is poured out, added the sherwood oil of 60～90 ℃ of 20mL, boiling range again, pour out sherwood oil behind the ultrasonic 40min, so repeat to extract 3 times.
(5) filter paper packet is taken out, put into 70 ℃ of baking ovens filter paper packet is dried to constant weight, weighing, recording quality (g).
The ultrasonic quality of handling the back minimizing of filter paper packet is the quality of crude fat in the sample.
With content of crude fat such as following table in the bright capsicum of the inventive method and soxhlet extraction mensuration
| Numbering | Fresh and dried ratio | Crude fat (%) (the inventive method) | Crude fat (%) (soxhlet extraction) |
| 1 | 16.931 | 0.38±0.034 | 0.330±0.0400 |
| 2 | 5.191 | 2.25±0.24 | 2.140±0.209 |
| 3 | 9.12 | 1.89±0.17 | 1.797±0.180 |
| 4 | 15.469 | 0.49±0.061 | 0.493±0.027 |
| 5 | 11.299 | 1.25±0.15 | 1.061±0.051 |
| 6 | 11.804 | 0.79±0.043 | 0.708±0.023 |
| 7 | 9.047 | 0.69±0.051 | 0.686±0.028 |
| 8 | 10.620 | 1.50±0.18 | 1.311±0.125 |
| 9 | 12.722 | 1.29±0.13 | 1.241±0.133 |
By measurement result as can be known, the difference as a result of crude fat content does not have conspicuousness in the bright capsicum of the inventive method and soxhlet extraction mensuration.
Claims (2)
1. method of measuring fast crude fat content in the food is characterized in that realizing through the following steps successively:
(1) get food samples to be measured, the baking oven of putting into 95～105 ℃ after the pulverizing is dried to constant weight, gets the fresh and dried f of ratio with the quality before dry divided by dried quality;
(2) take by weighing the food samples quality m1 to be measured that is dried to constant weight, wrap into the quantitative filter paper that in 70 ℃ of baking ovens, is dried to constant weight quality m2;
(3) filter paper packet that will be surrounded by food samples to be measured is put into glass container, add sherwood oil, the mass volume ratio of food samples to be measured and sherwood oil is 1g:15～80mL in the filter paper packet, glass container is put into supersonic wave cleaning machine, be 50～150w at power, temperature is 30 ℃ of ultrasonic extraction 15～50min down, and sherwood oil is poured out, and same operation repeats to extract 3 times;
(4) filter paper packet is taken out, in 70 ℃ baking oven, be dried to constant weight quality m3, according to the crude fat content in the following formula calculation sample:
The crude fat content of sample (%)=
2. the method for crude fat content in a kind of quick mensuration food according to claim 1 is characterized in that the boiling range of the described sherwood oil of step (3) is 60～90 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111766174A (en) * | 2020-07-01 | 2020-10-13 | 广州市优百特饲料科技有限公司 | Method for extracting crude fat from microcapsule type fat powder and method for measuring content of crude fat |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101846611A (en) * | 2010-06-03 | 2010-09-29 | 西北农林科技大学 | Method for determining oil content of vegetable oil material based on ultrasonic assistant extraction |
| CN102252936A (en) * | 2011-04-29 | 2011-11-23 | 山东省农业科学院农产品研究所 | Method for detecting crude fat in food |
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- 2013-05-24 CN CN2013101973189A patent/CN103278420A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101846611A (en) * | 2010-06-03 | 2010-09-29 | 西北农林科技大学 | Method for determining oil content of vegetable oil material based on ultrasonic assistant extraction |
| CN102252936A (en) * | 2011-04-29 | 2011-11-23 | 山东省农业科学院农产品研究所 | Method for detecting crude fat in food |
Non-Patent Citations (1)
| Title |
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| 张领弟 等: "超声波震荡快速测定肉与肉制品中游离脂肪的含量", 《疾病监测与控制杂志》, vol. 7, no. 4, 30 April 2013 (2013-04-30) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111766174A (en) * | 2020-07-01 | 2020-10-13 | 广州市优百特饲料科技有限公司 | Method for extracting crude fat from microcapsule type fat powder and method for measuring content of crude fat |
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Application publication date: 20130904 |