CN106092818A - The assay method of natural rubber content in a kind of seeds of rubber tree oil - Google Patents
The assay method of natural rubber content in a kind of seeds of rubber tree oil Download PDFInfo
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- CN106092818A CN106092818A CN201610721886.8A CN201610721886A CN106092818A CN 106092818 A CN106092818 A CN 106092818A CN 201610721886 A CN201610721886 A CN 201610721886A CN 106092818 A CN106092818 A CN 106092818A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The present invention discloses the assay method of natural rubber content in a kind of seeds of rubber tree oil, saponification is carried out after being mixed with alkali liquor by seeds of rubber tree oil, sterol therein, vitamin and some Hydrocarbon etc. can not be dissolved in hot ethanol with the material of alkali reflection, natural rubber can separate out with the form of micelle, with petroleum ether or normal hexane, rubber is dissolved again, dehydrated alcohol separates out again, thoroughly removes the impurity such as the saponified and non-saponifiable matter that is wrapped in natural rubber, obtains pure natural rubber.The present invention need not use main equipment, and simple to operate, condition easily reaches, low cost, and the laboratory of generic condition can realize；Accuracy is high, feasibility is strong, uses petroleum ether or normal hexane to carry out resuspended to rubber, is removed by the impurity such as the saponified or non-saponifiable matter wrapped up in rubber, it is ensured that the purity of natural rubber.
Description
Technical field
The present invention relates to the assay method of natural rubber content in a kind of seeds of rubber tree oil.
Background technology
Seeds of rubber tree oil be Brazil para ruber (Hevea brasiliensis) seed, through squeezing, refine
After the oils and fats that obtains, be a kind of rare torrid zone woody oleiferous plants.Seeds of rubber tree oil has the highest nutritive value, wherein linolenic acid
Content is 20.81%, linoleic acid content is 35.77%, is essential fatty acid, and existing seeds of rubber tree oil has become high-quality
Edible vegetable oil, slowly starts to come into huge numbers of families.Natural rubber is that monomer isoprene is through the producing high-molecular being polymerized
Compound, is widely present in vegetable food raw material, is the food additive in the legal gel-based candy of China.Although natural rubber
To human body non-hazardous, but the existence of natural rubber can affect the quality of edible seeds of rubber tree oil, therefore, at seeds of rubber tree
The refining process of oil can be removed.
In existing seeds of rubber tree oil, the detection method of natural rubber is patent 200810131054.6 " a kind of mensuration rubber
The method of natural rubber content in glue seed oil ", its detection method is the saponification utilizing oils and fats, by natural rubber soap therein
Dissolve, then natural rubber is scraped from flask, gauze carries out kneading cleaning, then carry out drying and weigh.The method
It is disadvantageous in that: one, natural rubber is in saponification process, can be by saponified miscellaneous with non-saponifiable matter etc. while separating out rubber
Matter is wrapped among rubber micelle, is only cleaned by kneading, will not be by rubber wash clean；Two, natural rubber has viscosity, by it
Scrape from flask walls, the loss of rubber mass can be caused first, second add experiment difficulty.
Therefore, it is necessary to existing detection method is improved, on the basis of ensureing accuracy in detection, reduce experiment difficulty
Degree, simplifies experiment condition.
Summary of the invention
For solving the weak point of existing detection method, the present invention provides natural rubber content in a kind of seeds of rubber tree oil
Assay method, the method is simple to operate, accuracy is high, low cost.
The present invention is realized by following technical proposal: the assay method of natural rubber content in a kind of seeds of rubber tree oil,
Through following each step:
(1) sample weighs
The flask being dried to constant weight is weighed by analytical balance, and bottle is heavily recorded as m1, it is accurate to 0.1mg；
Weigh 50～100g seeds of rubber tree oil with electronic scale, be recorded as m2, it is accurate to 0.01g, reinstalls in flask；
(2) saponification
Injecting 200～400mL potassium hydroxide-ethanol solution in flask, be connected with flask by reflux condensing tube, water-bath is 90
～at 95 DEG C, keep constant temperature, carry out refluxing 60～120min；
(3) clean
Take out flask, topple over saponification liquor while hot, rotate with 100～200mL distilled water and clean once, more anhydrous with 50～100mL
Ethanol purge twice；
(4) rubber is resuspended
In flask, add 10～20mL petroleum ether or n-hexane dissolution natural rubber, be subsequently adding 100～200mL dehydrated alcohol
Resuspended, make natural rubber again separate out；This step comes again；
(5) drying is weighed
Being put into by flask and dry 60～120min in thermostatic drying chamber, baking temperature is 103 DEG C+2 DEG C, take out flask after drying and put
Enter in exsiccator (built-in water suction variable color silica gel), be cooled to room temperature, and weigh with analytical balance, be recorded as m3, it is accurate to
0.1mg；
(6) rubber content calculates:
X is the content of natural rubber in sample, and unit is %；
m1For flask weight, unit is g；
m2For weighing oil weight, unit is g；
m3For flask and rubber gross weight, unit is g.
In the potassium hydroxide-ethanol solution of described step 2, the concentration of potassium hydroxide is 1～3.5mol/L.
The present invention can occur saponification according to for seeds of rubber tree oil in alkali liquor, and natural rubber belongs to hydro carbons, no
Can be saponified, thus can separate out from solution, by cleaning, dissolving, the step such as precipitation it is purified, thus survey natural
The content of rubber.Concrete, the present invention carries out saponification, sterol therein, vitamin after being mixed with alkali liquor by seeds of rubber tree oil
Can not be dissolved in hot ethanol with the material of alkali reflection with some Hydrocarbon etc., natural rubber can be analysed with the form of micelle
Going out, then dissolve rubber with petroleum ether (or normal hexane), dehydrated alcohol separates out again, thoroughly removes and is wrapped in natural rubber
In the impurity such as saponified and non-saponifiable matter, obtain pure natural rubber.
Advantages of the present invention:
A, simple to operate.The present invention need not use main equipment, and simple to operate, condition easily reaches, low cost, generic condition
Laboratory can realize.
B, accuracy are high, feasibility is strong.This method uses petroleum ether (or normal hexane) to carry out resuspended to rubber, by rubber
The impurity such as the saponified or non-saponifiable matter of parcel are removed, it is ensured that the purity of natural rubber.
Detailed description of the invention
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) sample weighs
The flask being dried to constant weight is weighed by analytical balance, and bottle is heavily recorded as m1=163.1239g, is accurate to 0.1mg；
Weigh seeds of rubber tree oil with electronic scale, be recorded as m2=49.60g, is accurate to 0.01g, reinstalls in flask；
(2) saponification
200mL potassium hydroxide-ethanol solution (wherein the concentration of potassium hydroxide is 1mol/L) is injected, by reflux condensation mode in flask
Pipe is connected with flask, and water-bath keeps constant temperature at 95 DEG C, carries out the 60min that refluxes；
(3) clean
Take out flask, topple over saponification liquor while hot, rotate with 100mL distilled water and clean once, then with 50mL washes of absolute alcohol two
Secondary；
(4) rubber is resuspended
In flask, add 10mL petroleum ether dissolution natural rubber, be subsequently adding 100mL dehydrated alcohol resuspended, make natural rubber weight
New precipitation；This step comes again；
(5) drying is weighed
Flask is put into drying 60min in thermostatic drying chamber, and baking temperature is 101 DEG C, takes out flask and put into exsiccator after drying
In (built-in water suction variable color silica gel), it is cooled to room temperature, and weighs with analytical balance, be recorded as m3=163.1726g, is accurate to
0.1mg；
(6) rubber content calculates:
X is the content of natural rubber in sample, and unit is %；
m1For flask weight, unit is g；
m2For weighing oil weight, unit is g；
m3For flask and rubber gross weight, unit is g.
Embodiment 2
(1) sample weighs
The flask being dried to constant weight is weighed by analytical balance, and bottle is heavily recorded as m1=182.8558g, is accurate to 0.1mg；
Weigh seeds of rubber tree oil with electronic scale, be recorded as m2=100.20g, is accurate to 0.01g, reinstalls in flask；
(2) saponification
400mL potassium hydroxide-ethanol solution (wherein the concentration of potassium hydroxide is 1.34mol/L) is injected in flask, will backflow
Condensing tube is connected with flask, and water-bath keeps constant temperature at 90 DEG C, carries out the 120min that refluxes；
(3) clean
Take out flask, topple over saponification liquor while hot, rotate with 200mL distilled water and clean once, then with 100mL washes of absolute alcohol two
Secondary；
(4) rubber is resuspended
In flask, add 20mL petroleum ether dissolution natural rubber, be subsequently adding 200mL dehydrated alcohol resuspended, make natural rubber weight
New precipitation；This step comes again；
(5) drying is weighed
Flask is put into drying 120min in thermostatic drying chamber, and baking temperature is 105 DEG C, takes out flask and put into exsiccator after drying
In (built-in water suction variable color silica gel), it is cooled to room temperature, and weighs with analytical balance, be recorded as m3=182.9594g, is accurate to
0.1mg；
(6) rubber content calculates:
X is the content of natural rubber in sample, and unit is %；
m1For flask weight, unit is g；
m2For weighing oil weight, unit is g；
m3For flask and rubber gross weight, unit is g.
Precision detects
Take Xishuangbanna Hua Kun biotechnology Co., Ltd produce hot moulding seeds of rubber tree oil crude oil (lot number:
20151230) 1000g, is divided into 10 parts, every part of 100g.
One, using the method for the present invention to detect the natural rubber content in this sample, result is as follows:
Upper table understands, and the rubber content of the seeds of rubber tree oil crude oil of hot moulding method squeezing is 0.1015 ± 0.0036%, the coefficient of variation
(CV): 3.591%.
Two, the method using patent 200810131054.6 " a kind of method measuring content of natural rubber in rubber seed oil "
Detecting, result is as follows:
Upper table understands, and utilizes the side of patent 200810131054.6 " a kind of method measuring content of natural rubber in rubber seed oil "
Method detects, and in the seeds of rubber tree oil of physical refining, natural rubber content is 0.1387 ± 0.0061%, the coefficient of variation
(CV): 4.379%.
Accuracy detects
Take concentration known 0.05% soybean oil (being dissolved in 999.5g soybean oil with natural rubber 0.5g) 1000g, be divided into 10 parts,
Every part of 100g.
One, using the inventive method to detect the natural rubber content in this sample, result is as follows:
Visible, the concentration of sample natural rubber is 0.05%, and measured value is 0.0505 ± 0.0015%, the coefficient of variation (CV):
2.908%。
Two, the method using patent 200810131054.6 " a kind of method measuring content of natural rubber in rubber seed oil "
Detecting, result is as follows:
The method utilizing patent 200810131054.6 " a kind of method measuring content of natural rubber in rubber seed oil " detects
In sample, the content of natural rubber is 0.0515 ± 0.0045%, the coefficient of variation (CV): 8.66%.
Claims (2)
1. the assay method of natural rubber content in a seeds of rubber tree oil, it is characterised in that through following each step:
(1) sample weighs
The flask being dried to constant weight is weighed by analytical balance, and bottle is heavily recorded as m1, it is accurate to 0.1mg；
Weigh 50～100g seeds of rubber tree oil with electronic scale, be recorded as m2, it is accurate to 0.01g, reinstalls in flask；
(2) saponification
Injecting 200～400mL potassium hydroxide-ethanol solution in flask, be connected with flask by reflux condensing tube, water-bath is 90
～at 95 DEG C, keep constant temperature, carry out refluxing 60～120min；
(3) clean
Take out flask, topple over saponification liquor while hot, rotate with 100～200mL distilled water and clean once, more anhydrous with 50～100mL
Ethanol purge twice；
(4) rubber is resuspended
In flask, add 10～20mL petroleum ether or n-hexane dissolution natural rubber, be subsequently adding 100～200mL dehydrated alcohol
Resuspended, make natural rubber again separate out；This step comes again；
(5) drying is weighed
Being put into by flask and dry 60～120min in thermostatic drying chamber, baking temperature is 103 DEG C+2 DEG C, take out flask after drying and put
Enter in exsiccator, be cooled to room temperature, and weigh with analytical balance, be recorded as m3, it is accurate to 0.1mg；
(6) rubber content calculates:
X is the content of natural rubber in sample, and unit is %；
m1For flask weight, unit is g；
m2For weighing oil weight, unit is g；
m3For flask and rubber gross weight, unit is g.
The assay method of natural rubber content in seeds of rubber tree oil the most according to claim 1, it is characterised in that: described
In the potassium hydroxide-ethanol solution of step 2, the concentration of potassium hydroxide is 1～3.5mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610721886.8A CN106092818A (en) | 2016-08-25 | 2016-08-25 | The assay method of natural rubber content in a kind of seeds of rubber tree oil |
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| CN201610721886.8A CN106092818A (en) | 2016-08-25 | 2016-08-25 | The assay method of natural rubber content in a kind of seeds of rubber tree oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109793788A (en) * | 2017-11-16 | 2019-05-24 | 徐爽 | A kind of substance of reducing blood lipid, using and preparation method thereof |
| CN110179850A (en) * | 2018-02-23 | 2019-08-30 | 徐爽 | A kind of substance is being alleviated and the application on treatment perimenopausal syndrome |
Citations (8)
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|---|---|---|---|---|
| JPS5433785A (en) * | 1977-08-19 | 1979-03-12 | Tokico Ltd | Measurement of chlorine content in vulcanized rubber |
| US4681996A (en) * | 1982-12-16 | 1987-07-21 | Cem Corporation | Analytical process in which materials to be analyzed are directly and indirectly heated and dried by microwave radiation |
| CN1054985A (en) * | 1990-03-15 | 1991-10-02 | 中国科学院化学研究所 | Comprehensive extraction of gutta-percha |
| CN1215059A (en) * | 1997-10-18 | 1999-04-28 | 李世泰 | Extration of steroid compound from rubber seeds |
| CN1445347A (en) * | 2000-04-20 | 2003-10-01 | 陈瑞恭 | Method for extracting oil of rubber seeds |
| CN101650288A (en) * | 2008-08-14 | 2010-02-17 | 海南省粮油科学研究所 | Method for determining content of natural rubber in rubber seed oil |
| CN102807678A (en) * | 2011-06-02 | 2012-12-05 | 中国科学院化学研究所 | Method for circularly and continuously extracting eucommia gum, eucommia seed oil, eucommia extractum and eucommia resin from eucommia seeds |
| CN105524713A (en) * | 2016-02-03 | 2016-04-27 | 西双版纳华坤生物科技有限责任公司 | Industrialized method for removing rubber in rubber tree seed oil |
-
2016
- 2016-08-25 CN CN201610721886.8A patent/CN106092818A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5433785A (en) * | 1977-08-19 | 1979-03-12 | Tokico Ltd | Measurement of chlorine content in vulcanized rubber |
| US4681996A (en) * | 1982-12-16 | 1987-07-21 | Cem Corporation | Analytical process in which materials to be analyzed are directly and indirectly heated and dried by microwave radiation |
| CN1054985A (en) * | 1990-03-15 | 1991-10-02 | 中国科学院化学研究所 | Comprehensive extraction of gutta-percha |
| CN1215059A (en) * | 1997-10-18 | 1999-04-28 | 李世泰 | Extration of steroid compound from rubber seeds |
| CN1445347A (en) * | 2000-04-20 | 2003-10-01 | 陈瑞恭 | Method for extracting oil of rubber seeds |
| CN101650288A (en) * | 2008-08-14 | 2010-02-17 | 海南省粮油科学研究所 | Method for determining content of natural rubber in rubber seed oil |
| CN102807678A (en) * | 2011-06-02 | 2012-12-05 | 中国科学院化学研究所 | Method for circularly and continuously extracting eucommia gum, eucommia seed oil, eucommia extractum and eucommia resin from eucommia seeds |
| CN105524713A (en) * | 2016-02-03 | 2016-04-27 | 西双版纳华坤生物科技有限责任公司 | Industrialized method for removing rubber in rubber tree seed oil |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109793788A (en) * | 2017-11-16 | 2019-05-24 | 徐爽 | A kind of substance of reducing blood lipid, using and preparation method thereof |
| CN110179850A (en) * | 2018-02-23 | 2019-08-30 | 徐爽 | A kind of substance is being alleviated and the application on treatment perimenopausal syndrome |
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Application publication date: 20161109 |