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Ultrasonic extraction method of heavy metal elements in vegetables

An extraction method and heavy metal technology, which is applied in the field of ultrasonic extraction of chromium, lead, cadmium, nickel, and zinc five heavy metal elements in vegetables, can solve the problem of less application of heavy metal extraction, and reduce the emission of toxic, harmful and corrosive gases , The reaction is mild and safe, and the effect of less reagent consumption

Inactive Publication Date: 2015-02-25
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ultrasonic extraction is widely used in the extraction of active ingredients of Chinese medicinal materials, animals and plants, but less in the extraction of heavy metals in food

Method used

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  • Ultrasonic extraction method of heavy metal elements in vegetables
  • Ultrasonic extraction method of heavy metal elements in vegetables
  • Ultrasonic extraction method of heavy metal elements in vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Take GBW10015 spinach, rinse it with running water first, then wash it with distilled water and deionized water, air-dry it, weigh it, and dry it in an oven at 60°C for 72 hours. The dried sample is homogenized with an agate mortar and passed through 200 mesh (74μm) Sieve and store in a polyethylene bottle in a desiccator at room temperature for later use.

[0038] (2) Wet digestion method: Weigh 1.0g of the sample into a tall beaker, put a few glass beads, add 10mL of 65% HNO 3 -70% HClO 4 (9:1, V / V) cover and soak overnight, heat and digest on the electric heating plate, if it turns brown-black, add mixed acid until white smoke, until the digestive juice is colorless, transparent or slightly yellow, and the excess The acid was evaporated to nearly dryness, cooled, and the digestive juice was washed into a 25mL volumetric flask with a dropper, and the tall beaker was washed several times with a small amount of water. Blank test.

[0039] (3) Ultrasonic extractio...

Embodiment 2

[0042] (1) Take spinach, rinse it with running water first, then wash it with distilled water and deionized water, air-dry it, weigh it, and dry it in an oven at 70°C for 48 hours. The dried sample is homogenized with an agate mortar and passed through a 150-mesh (104 μm) sieve , stored in a polyethylene bottle in a desiccator at room temperature for later use.

[0043] (2) Dry ashing: Weigh 1.0g of the sample into a porcelain crucible, add 1mL of phosphoric acid (1+10), soak for more than 1h, place the crucible on a heating plate, carbonize on low heat until smokeless, and then transfer it into a muffle furnace In medium temperature, ash at 500±25°C for about 8 hours, until the sample is grayish white, take it out and let it cool, then add a small amount of hydrochloric acid (1+11), heat on low heat, do not make it dry, add a little mixed acid if necessary, and repeat the treatment like this , until there is no carbon particle in the residue, add 10mL hydrochloric acid (1+11)...

Embodiment 3

[0047] (1) Take samples of celery, cabbage, leek and garlic sprouts, rinse them with running water first, then wash them with distilled water and deionized water, air-dry them, weigh them, and dry them in an oven at 65°C for 60 hours. The dried samples are homogenized with an agate mortar. Pass through a 170-mesh (88 μm) sieve, and store in a polyethylene bottle in a desiccator at room temperature for later use.

[0048] (2) Microwave digestion method: Weigh 0.5g of the sample into a polytetrafluoroethylene digestion tank, add 5mL of 65% nitric acid and 1mL of 30% hydrogen peroxide, place it in a microwave digestion device, and digest according to the program: 0.2MPa, 2min; 0.5 MPa, 2min; 1.0MPa, 2min; 1.5MPa, 5min; 2.0MPa, 5min; cooling for 10min. After the digestion is completed, cool to room temperature, heat on an electric heating plate until nearly dry, and dilute the solution in a 50-100mL volumetric flask after cooling. At the same time as a blank test.

[0049] (3) U...

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Abstract

The invention discloses an ultrasonic extraction method of heavy metal elements in vegetables. The ultrasonic extraction method comprises the following steps: firstly, rinsing a sample thoroughly with water, next, washing with distilled water and deionized water, air-drying, weighing, drying in a drying oven, homogenizing the dried sample by use of agate mortar, sieving, and preserving in a dryer at normal temperature in a polyethylene bottle for later use; weighing 0.1g of the treated vegetable sample and putting the sample into a centrifugal tube, adding an acidic extracting agent, putting into ultrasonic bath for ultrasonic extraction, centrifuging and separating out the supernatant; cleaning the residue by use of ultrapure water before ultrasonic extraction and centrifuging, also taking the supernatant for blending with the acid extract, preserving in the polyethylene bottle at 4 DEG C for later use after the volume is constant, and then measuring the content of each element of Cd, Cr, Ni, Pb and Zn by virtue of atomic absorption spectrophotometry. According to the ultrasonic extraction method of heavy metal elements in vegetables, a pretreatment method for ultrasonically extracting heavy metal elements in vegetables is established and has the advantages of simplicity and quickness, high recovery rate, good safety, low pollution, low reagent consumption, low residue and the like.

Description

technical field [0001] The invention relates to the technical field of heavy metal pretreatment methods, in particular to an ultrasonic extraction method for five heavy metal elements including cadmium, chromium, nickel, lead and zinc in vegetables. Background technique [0002] The determination methods of heavy metal elements such as atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, etc. usually require the digestion of solid samples. The commonly used digestion methods include dry ashing, wet digestion, microwave Digestion etc. However, the dry ashing method takes a long time, usually 6 to 14 hours, and has strict requirements on the ashing temperature. If the ashing temperature is too low, the organic matter cannot be completely decomposed, and if the ashing temperature is too high, it will easily cause the The loss of elements; the wet digestion method is usually carried out on a heati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40
Inventor 赵刚顾佳丽励建荣夏云生白凤翎包德才
Owner BOHAI UNIV
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