CN105136932A - Determination method of natural vitamin E content in sunflower oil - Google Patents
Determination method of natural vitamin E content in sunflower oil Download PDFInfo
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- CN105136932A CN105136932A CN201510565653.9A CN201510565653A CN105136932A CN 105136932 A CN105136932 A CN 105136932A CN 201510565653 A CN201510565653 A CN 201510565653A CN 105136932 A CN105136932 A CN 105136932A
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Abstract
The invention relates to a field of the natural product content determination, and concretely relates to a determination method of natural vitamin E content in sunflower oil. An extraction condition of the natural vitamin E is optimized by using an ultrasonic method, the content of the natural vitamin E in the sunflower oil sample is determined by using a HPLC method, thereby providing reference for plant oil quality standards. The invention has the advantages of simple step, economic utility and easy 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 sunflower 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.
Sunflower oil is the oil extracted from sunflower seeds, and because it is nutritious, a lot of national people like to eat in the world, some titles it be healthy oil, oil of lengthening the life.
Sunflower oil is with the famous health-care edible oil of the linoleic acid of high-load.In 21 century, cardiovascular and cerebrovascular disease such as the diseases such as coronary heart disease, headstroke, cerebral thrombus, artery sclerosis, hypertension increase, and long-term edible suitable oil and fat product, can have greatly improved to above-mentioned symptom.Sunflower oil is exactly one very outstanding in healthy grease, and the many local sunflower oils in the present world have become the first-selection oil of consumer and cook, and sunflower oil consumption figure worldwide ranks the 3rd in all vegetable oil.
Sunflower oil contains the multiple materials useful to the mankind such as sterol, vitamin, linoleic acid, and wherein natural tocopherol level content in all main plant oil is the highest; And linoleic acid content can reach about 70%.Sunflower oil can reduce cholesterol in serum level, reduces triglyceride levels, has the effect reduced blood pressure.And sunflower oil light transparent, culinary art time can retain wholefood local flavor, its smoke point is also very high, can exempt the harm of oil smoke to human body.
At present, the analytical approach of vitamin E 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 sunflower 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 sunflower 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 sunflower oil, it is characterized in that comprising the following steps:
(1) take: count by weight, get 1 part, sunflower oil sample, accurately weighed;
(2) ultrasonic extraction: add 2 ~ 3 parts of extracted by ether agent, 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 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 sunflower 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 sunflower oil, comprise the following steps:
(1) take: count by weight, get 1 part, sunflower oil sample, accurately weighed;
(2) ultrasonic extraction: add 2 ~ 3 parts of extracted by ether agent, ultrasonic extraction 20 ~ 25min, 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, and mobile phase and water volume ratio are 95:2, isocratic elution 18min, flow control 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 sunflower 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 sunflower oil, it is characterized in that comprising the following steps:
(1) take: count by weight, get 1 part, sunflower oil sample, accurately weighed;
(2) ultrasonic extraction: add 2 ~ 3 parts of extracted by ether agent, 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 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 sunflower oil sample, calculate the content of vitamin E.
2. a kind of assay method detecting natural tocopherol level in sunflower 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 sunflower 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 (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106018647A (en) * | 2016-07-11 | 2016-10-12 | 吉林益民堂制药有限公司 | Method for establishing sunflower plate HPLC standard fingerprint |
Citations (2)
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CN104090044A (en) * | 2014-07-16 | 2014-10-08 | 中国农业科学院油料作物研究所 | Method for analyzing fatty acid composition in edible vegetable oil and true and false identification method of edible vegetable oil based on fatty acid composition |
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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CN104090044A (en) * | 2014-07-16 | 2014-10-08 | 中国农业科学院油料作物研究所 | Method for analyzing fatty acid composition in edible vegetable oil and true and false identification method of edible vegetable oil based on fatty acid composition |
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 (3)
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CN106018647A (en) * | 2016-07-11 | 2016-10-12 | 吉林益民堂制药有限公司 | Method for establishing sunflower plate HPLC standard fingerprint |
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