CN105116073A - Determination method for detecting content of natural vitamin E in palm oil - Google Patents
Determination method for detecting content of natural vitamin E in palm oil Download PDFInfo
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- CN105116073A CN105116073A CN201510565894.3A CN201510565894A CN105116073A CN 105116073 A CN105116073 A CN 105116073A CN 201510565894 A CN201510565894 A CN 201510565894A CN 105116073 A CN105116073 A CN 105116073A
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Abstract
The invention relates to the field of determination of the content of natural products and particularly relates to a determination method for detecting the content of natural vitamin E in palm oil. Extraction conditions of the natural vitamin E are optimized by adopting an ultrasonic method, and the content of the natural vitamin E in a palm oil sample is determined by adopting a high performance liquid chromatography, so as to provide reference to plant oil quality standards. The determination method has simple steps, is economical and practical and is applicable to popularization.
Description
Technical field
The present invention relates to natural products assay field, be specially a kind of assay method detecting natural tocopherol level in palm oil.
Background technology
Natural VE (VitaminE) is a kind of liposoluble vitamin, also known as tocopherol, is one of topmost antioxidant.Be dissolved in the organic solvents such as fat and ethanol, water insoluble, heat, acid are stablized, unstable to alkali, responsive to oxygen, insensitive to heat, but time fried, Vitamin E activity obviously reduces.Tocopherol can promote that sex hormone is secreted, and man's sperm motility and quantity are increased; Woman's female hormone concentration is increased, and improve fecundity, prevention of miscarriage, also can be used for preventing and treating the aspects such as male sterility, burn, frostbite, capillary hemorrhage, climacteric syndrome, beauty treatment has good curative effect.Also found that vitamin E can suppress the lipid peroxidation in eye lens to react, and made end slightly blood vessel dilatation, improves blood circulation in recent years.
Each vegetable oil is one of main source obtaining natural VE in people's daily life, in the vegetable oil of different cultivars, the content of natural VE has larger difference, and therefore the composition of natural VE and content can as of edible vegetable oil and fat quality important evaluation indexes.
In vegetable oil, palm oil is also referred to as saturated grease, because it contains the saturated fat of 50%.Grease is saturated fat, monounsaturated fatty acid, polyunsaturated fat three kinds of composition mixing formations.Human body is to palmitic absorption and digestion rate more than 97%, and the same with other all vegetable edible oils, palm oil itself is not containing cholesterol.
As the grease that a species saturation is higher, palm oil was once inferred likely can increase cholesterol level in human serum.But through the further experimental demonstration of many experts, find that edible palm oil not only can not increase the cholesterol in serum, there is the trend reducing cholesterol on the contrary, reason is the display of a large amount of data, the impact of different saturated fatty acids on blood fat is different, neutral fat acid is rich in palm oil, the material impelling cholesterol to improve content in palm oil very little (1%), the natural vitamin e be rich in palm oil and tocotrienol (600-1000mg/kg), carotenoid (500-700mg/kg) and linoleic acid (10%) very useful to the health of human body.Some researchists once studied respectively for different ethnic groups (Europe, America, Asia), and result shows that palm oil is a kind of edible vegetable oil meeting health needs completely.
At present, the analytical approach of tocopherol comprises high performance liquid chromatography, vapor-phase chromatography, thin-layered chromatography, paper chromatography, column chromatography, colourimetry etc., and the most frequently used is high performance liquid chromatography, and China's existing national standards, industry standard all adopt this method.These standards all have employed method for saponification and extract before liquid-phase chromatographic analysis, and the method time is long and step is complicated.
Summary of the invention
The object of the invention is to now provide a kind of assay method detecting natural tocopherol level in palm oil, the extraction conditions of ultrasonic method to natural VE is adopted to be optimized, and adopt the content of natural VE in high effective liquid chromatography for measuring palm oil sample, for Vegetable Oil Quality standard provides reference, step of the present invention is simple, economical and practical, be suitable for promoting.
For realizing the object of the invention, the technical scheme of employing is:
Detect an assay method for natural tocopherol level in palm oil, it is characterized in that comprising the following steps:
(1) take: count by weight, get 1 part, palm oil sample, accurately weighed;
(2) ultrasonic extraction: add 1.2 ~ 1.3 parts of methyl alcohol, ultrasonic extraction 20 ~ 25min, pours out collection by supernatant;
(3) step (2) 1 ~ 2 times are repeated;
(4) concentrated: by supernatant collection, to be concentrated into dry, to obtain sample extracting solution;
(5) measure: high-performance liquid chromatogram determination, adopt C18 chromatographic column, column temperature controls at 32 ~ 34 DEG C, mobile phase methanol and water volume ratio are 95:1.8 ~ 2.0, isocratic elution 16 ~ 18min, and flow control is at 1.1 ~ 1.3mL/min, diode array detector determined wavelength 295nm, sample size 20 μ L;
The preparation of reference substance solution: get vitamin E reference substance, makes the reference substance solution of every 1ml containing 3 μ g, 6 μ g, 12 μ g, 30 μ g, 60 μ g;
High performance liquid chromatography: the reference substance solution of variable concentrations is respectively with 20 μ L sample introductions, record the peak area of vitamin E under 295nm wavelength, with each standard reference material peak area of gained for ordinate, each corresponding standard reference material concentration is that horizontal ordinate does typical curve respectively, calculates the equation of linear regression of vitamin E respectively; Then high-performance liquid chromatogram determination is carried out to sample extraction liquor, obtain the peak area of vitamin E under 295nm wavelength, according to the content of vitamin E in respective typical curve calculation sample extract, and in conjunction with the quality of palm oil sample, calculate the content of vitamin E.
Further, the middle flow control of described step (5) is at 1.2mL/min.
Further, described step (5) center pillar temperature control is at 33 DEG C.
The invention has the beneficial effects as follows:
One, ultrasound wave extract yield of the present invention is high, measures relative deviation little, has good accuracy and precision to the mensuration of vitamin E.
Two, step of the present invention is comparatively simple, and adopt compared with saponification in the world, and contracting ovum detection test specimen, is more suitable for grain and oil relevant enterprise and carries out qualitative control greatly.
Embodiment
Be described in further detail below by specific embodiment.
Embodiment 1
Detect an assay method for natural tocopherol level in palm oil, comprise the following steps:
(1) take: count by weight, get 1 part, palm oil sample, accurately weighed;
(2) ultrasonic extraction: add 1.25 parts of methyl alcohol, ultrasonic extraction 20min, pours out collection by supernatant;
(3) step (2) 2 times are repeated;
(4) concentrated: by supernatant collection, to be concentrated into dry, to obtain sample extracting solution;
(5) measure: high-performance liquid chromatogram determination, adopt C18 chromatographic column, column temperature controls at 33 DEG C, mobile phase methanol and water volume ratio are 95:2, isocratic elution 18min, and flow control is at 1.2mL/min, diode array detector determined wavelength 295nm, sample size 20 μ L;
The preparation of reference substance solution: get vitamin E reference substance, makes the reference substance solution of every 1ml containing 3 μ g, 6 μ g, 12 μ g, 30 μ g, 60 μ g;
High performance liquid chromatography: the reference substance solution of variable concentrations is respectively with 20 μ L sample introductions, record the peak area of vitamin E under 295nm wavelength, with each standard reference material peak area of gained for ordinate, each corresponding standard reference material concentration is that horizontal ordinate does typical curve respectively, calculates the equation of linear regression of vitamin E respectively; Then high-performance liquid chromatogram determination is carried out to sample extraction liquor, obtain the peak area of vitamin E under 295nm wavelength, according to the content of vitamin E in respective typical curve calculation sample extract, and in conjunction with the quality of palm oil sample, calculate the content of vitamin E.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. detect an assay method for natural tocopherol level in palm oil, it is characterized in that comprising the following steps:
(1) take: count by weight, get 1 part, palm oil sample, accurately weighed;
(2) ultrasonic extraction: add 1.2 ~ 1.3 parts of methyl alcohol, ultrasonic extraction 20 ~ 25min, pours out collection by supernatant;
(3) step (2) 1 ~ 2 times are repeated;
(4) concentrated: by supernatant collection, to be concentrated into dry, to obtain sample extracting solution;
(5) measure: high-performance liquid chromatogram determination, adopt C18 chromatographic column, column temperature controls at 32 ~ 34 DEG C, mobile phase methanol and water volume ratio are 95:1.8 ~ 2.0, isocratic elution 16 ~ 18min, and flow control is at 1.1 ~ 1.3mL/min, diode array detector determined wavelength 295nm, sample size 20 μ L;
The preparation of reference substance solution: get vitamin E reference substance, makes the reference substance solution of every 1ml containing 3 μ g, 6 μ g, 12 μ g, 30 μ g, 60 μ g;
High performance liquid chromatography: the reference substance solution of variable concentrations is respectively with 20 μ L sample introductions, record the peak area of vitamin E under 295nm wavelength, with each standard reference material peak area of gained for ordinate, each corresponding standard reference material concentration is that horizontal ordinate does typical curve respectively, calculates the equation of linear regression of vitamin E respectively; Then high-performance liquid chromatogram determination is carried out to sample extraction liquor, obtain the peak area of vitamin E under 295nm wavelength, according to the content of vitamin E in respective typical curve calculation sample extract, and in conjunction with the quality of palm oil sample, calculate the content of vitamin E.
2. a kind of assay method detecting natural tocopherol level in palm oil according to claim 1, is characterized in that: in described step (5), flow control is at 1.2mL/min.
3. a kind of assay method detecting natural tocopherol level in palm oil according to claim 1, is characterized in that: described step (5) center pillar temperature control is at 33 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198826A (en) * | 2016-07-15 | 2016-12-07 | 江苏出入境检验检疫局动植物与食品检测中心 | By tocopherol and the method for tocotrienol content in gas chromatogram positive chemical source mass Spectrometry for Determination edible vegetable oil |
| CN108195956A (en) * | 2017-12-15 | 2018-06-22 | 广州中生生物技术有限公司 | The assay method of food vitamins E contents |
| CN110220995A (en) * | 2019-07-05 | 2019-09-10 | 浙江艾兰得生物科技有限公司 | The high-efficiency liquid chromatography method for detecting of content of vitamin E |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012099037A1 (en) * | 2011-01-17 | 2012-07-26 | 築野食品工業株式会社 | Analytical method for vitamin e |
| CN104569262A (en) * | 2014-12-30 | 2015-04-29 | 广州白云山汉方现代药业有限公司 | Method for simultaneously determining contents of alpha-tocopherol and squalene in multiple vegetable oils |
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2015
- 2015-09-08 CN CN201510565894.3A patent/CN105116073A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012099037A1 (en) * | 2011-01-17 | 2012-07-26 | 築野食品工業株式会社 | Analytical method for vitamin e |
| CN104569262A (en) * | 2014-12-30 | 2015-04-29 | 广州白云山汉方现代药业有限公司 | Method for simultaneously determining contents of alpha-tocopherol and squalene in multiple vegetable oils |
Non-Patent Citations (4)
| Title |
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| SASKIA FRANKE等: "Analysis of carotenoids and vitamin E in selected oilseeds,press cakes and oils", 《EUR. J. LIPID SCI. TECHNOL.》 * |
| 于瑞祥等: "反相高效液相色谱法同时测定植物油中四种生育酚", 《分析测试学报》 * |
| 寇立娟等: "反相高效液相色谱法快速测定植物油中的维生素E", 《中国食物与营养》 * |
| 李柰等: "食用植物油中生育酚含量测定方法优化及分析", 《食品科学技术学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198826A (en) * | 2016-07-15 | 2016-12-07 | 江苏出入境检验检疫局动植物与食品检测中心 | By tocopherol and the method for tocotrienol content in gas chromatogram positive chemical source mass Spectrometry for Determination edible vegetable oil |
| CN108195956A (en) * | 2017-12-15 | 2018-06-22 | 广州中生生物技术有限公司 | The assay method of food vitamins E contents |
| CN110220995A (en) * | 2019-07-05 | 2019-09-10 | 浙江艾兰得生物科技有限公司 | The high-efficiency liquid chromatography method for detecting of content of vitamin E |
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