Method for detecting d-alpha-tocopherol and 1-alpha-tocopherol in food through gas chromatography
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A gas chromatography and tocopherol technology, which is applied in the detection field, can solve the problems of l-α-tocopherol determination, difficult separation of different types, measurement interference, etc., and achieves the effects of good anti-specificity, easy operation and improved extraction rate.
Inactive Publication Date: 2014-01-01
ZANYU TECH GRP CO LTD
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Among these methods (1) Colorimetric method: This method is simple to operate and has high sensitivity; but since vitamin E has no specific reaction, some methods need to be used to remove interference
(2) Fluorescence method: This method has strong specificity, less interference, sensitive, fast and simple, but the analysis result is actually only the value of α-E
(4) Gas chromatography: Although this method can accurately quantify vitamin E at present, it is difficult to separate different types, and stearic substances such as cholesterol interfere with the determination
All the determination results of these methods are for the quantification of α-tocopherol, and the amount of d-α-tocopherol and l-α-tocopherol has not been effectively determined. At present, there is no detection of d-α-tocopherol in food Analytical Report on the Determination Method of Phenol
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[0024] The train of thought of the present invention is: adopt suitable sample pretreatment technology and capillary chromatographic separation column, weigh a certain amount of food in the saponification bottle, add ascorbic acid solution, potassium hydroxide solution and absolute ethanol in boiling water bath saponification backflow, then put Transfer the saponified solution into a separatory funnel, wash with water and petroleum ether, pass through an anhydrous sodium sulfate column, concentrate in a water bath and rotate until nearly dry, add methanol to dissolve, mix, and constant volume, then centrifuge and separate in a centrifuge, and take the supernatant for input Gas chromatography with a hydrogen flame detector. in:
[0025] (1) The first point of the method is that the sample is heated and saponified with potassium hydroxide-ethanol solution, and extracted with petroleum ether, which avoids the interference of the sample matrix on the chromatographic peak, removes ...
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Abstract
The invention relates to a method for detecting d-alpha-tocopherol and 1-alpha-tocopherol in food through gas chromatography and aims to provide a method which has the characteristics that the specificity is strong, the operation is simple and convenient, the anti-interference ability is good, and the accuracy is high, and the method is suitable for detecting of the content of the d-alpha-tocopherol and the 1-alpha-tocopherol in the food. The technical scheme of the method is as follows: the method for detecting the d-alpha-tocopherol and the 1-alpha-tocopherol in the food through the gas chromatography comprises the following steps: 1) a sample is prepared; 2) concentration is performed; 3) detection by an instrument is performed. Saponification bottle washing in the step 1) refers to that a saponification bottle is washed by 50 mL water for three times, and then the washing liquor is merged into a separating funnel; the saponification bottle and residues in the saponification bottle are washed by 100 mL petroleum ether twice; the petroleum ether liquid is merged into the separating funnel; the separating funnel is shook for 2 minutes, still standing is performed for layering, and a water layer is removed; the petroleum ether liquid in the separating funnel is washed by 50 mL distilled water, and a piece of pH test paper is used for detection until the water layer does not show alkalinity for standby application.
Description
technical field [0001] The invention relates to a detection method, in particular to a detection method for detecting d-alpha-tocopherol and l-alpha-tocopherol in food by gas chromatography. Background technique [0002] For most vitamins, natural vitamins and synthetic vitamins are not very different in chemical structure, biological activity, and absorption and utilization by the human body except for the difference in source, but vitamin E is an exception. Vitamin E, also known as tocopherol, its chemical structure is a derivative of Chroman. Vitamin E has 8 different isomers of α, β, γ, δ tocopherol and α, β, γ, δ tocotrienol, only α-tocopherol is industrially produced in natural and synthetic forms, the other three tocopherols β -, γ-, δ- are only in natural form, as are the four tocotrienols (α-, β-, γ-, δ-), there are no synthetic tocotrienols. [0003] Natural and synthetic are not only different in source, but also in molecular structure, biological activity, abso...
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