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An ionic liquid two-phase extraction/HPLC method for the detection of spices in rice
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An ionic liquid and two-phase technology, which is used in measurement devices, material separation, and analysis of materials, etc., can solve the problems of polluting the environment, many impurities, and increasing detection costs, and achieves the effects of environmental friendliness, high sensitivity, and easy operation.
Inactive Publication Date: 2016-08-17
SOUTH CHINA AGRI UNIV
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The solvent extraction method uses a large amount of organic solvents, which not only pollutes the environment, but also extracts more impurities, which affects the accuracy of detection
Although the solid-phase extraction method can reduce the interference of impurities, it needs to go through a series of steps such as the activation of small columns, the adsorption of target substances, the elution of impurities, and the elution of target substances. The operation is cumbersome and time-consuming, and it is not suitable for the processing of batch samples.
At the same time, due to the high price of commercial solid-phase extraction cartridges, the detection cost will be greatly increased.
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Embodiment 1
[0024] Screening of ionic liquid two-phase aqueous system:
[0025] In the pre-experiment process, the following types of ionic liquid two-phase aqueous systems were made: [Bmim]Cl / ammonium sulfate, [Bmim]Cl / sodium sulfate, [Bmim]Cl / sodium carbonate, [Bmim]Cl / Sodium Chloride, [Bmim]Cl / Dipotassium Hydrogen Phosphate, [Omim]Cl / Ammonium Sulfate, [Omim]Cl / Sodium Sulfate, [Omim]Cl / Sodium Carbonate, [Omim]Cl / Sodium Chloride, [Omim] Cl / dipotassium hydrogen phosphate, [Bmim]BF 4 / Ammonium sulfate, [Bmim] BF 4 / Sodium Sulfate, [Bmim] BF 4 / Sodium Carbonate, [Bmim] BF 4 / NaCl, [Bmim]BF 4 / dipotassium hydrogen phosphate, but only the [Bmim]Cl / dipotassium hydrogen phosphate aqueous two-phase system with the following composition is found: the mass fraction of [Bmim]Cl is 10~25%, and the mass fraction of dipotassium hydrogen phosphate is 30~50% %; suitable for the extraction of spices.
Embodiment 2
[0027] The rice of the present embodiment is common rice, a kind of method of ionic liquid two-phase extraction / HPLC detects spices in rice, and its specific steps are:
[0028] 1. Preparation of standard stock solutions of four spices (maltol, ethyl maltol, vanillin, ethyl vanillin): accurately weigh 0.0100 g (accurate to 0.0001 g) of pure standard substances in a small beaker , dissolved in 15% (V / V) acetonitrile solution and made to a 10 mL volumetric flask, and stored in a refrigerator at 4 °C for use.
[0029] 2. Sample pretreatment: first prepare an ionic liquid two-phase aqueous system with a total mass of 2 g. In this system, the mass of ionic liquid ([Bmim]) is 0.3 g (15%, w / w), dipotassium hydrogen phosphate 0.7 g (35%, w / w) of water has a mass of 1.0 g (50%, w / w). After the system is configured, add 0.2 g of rice products, shake and mix well, and place in a water bath at 40 °C for 15 minutes. Afterwards, the upper phase solution, that is, the ionic liquid phase, w...
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Abstract
The invention belongs to the technical field of food safety detection, and particularly discloses a method for detecting spices in rice by ionic liquid two-aqueous-phase extraction / high performance liquid chromatography (HPLC). The method comprises the following steps of firstly, extracting by using a [Bmim]Cl / dipotassium phosphate two-aqueous-phase system; then analyzing by combining the HPLC, wherein the mass fractions of the [Bmim]Cl and the dipotassium phosphate in the [Bmim]Cl / dipotassium phosphate two-aqueous-phase system are respectively 10-25% and 30-50%. The method has the advantages of being simple in detection steps, easy to operate, low in limit of detection, environmentally friendly and the like, thus having wider application prospect in the food detection field.
Description
technical field [0001] The invention relates to the technical field of food safety detection, in particular to a method for detecting spices in rice by ionic liquid two-phase extraction / HPLC. Background technique [0002] Rice is the staple food of more than two-thirds of the population in my country. With the improvement of people's living standards, higher requirements have been put forward for the edible quality of rice, and fragrant rice has been welcomed by consumers. However, at present, the total amount of fragrant rice cannot meet the needs of consumers, so some people use rice essence in the process of rice production and processing due to profit-driven, so as to pass off fragrant rice. What's more, rice essence is added to old rice to pretend to be new rice to deceive consumers. Relevant literature reports that the main components or ingredients of rice essence are propylene glycol, 2-acetylpyridine, vanillin, ethyl vanillin and ethyl maltol. Among them, vanilli...
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