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Pretreatment method for solid food sample based on ionic liquid

A technique for sample pretreatment and ionic liquids

Active Publication Date: 2019-12-13
武汉海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current method is not only time-consuming and labor-intensive, but also consumes a large amount of strong acid and strong oxidizing reagents, the treatment conditions are harsh, and a large amount of waste gas is generated, and it will bring great harm to the health of analysts and cause some pollution to the environment.
If not handled properly, there will be safety accidents
At the same time, the ash method, microwave digestion method or acid digestion method requires specific equipment, which increases the cost of sample pretreatment
[0004] Therefore, the current pretreatment methods for solid food samples still need to be improved

Method used

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  • Pretreatment method for solid food sample based on ionic liquid
  • Pretreatment method for solid food sample based on ionic liquid
  • Pretreatment method for solid food sample based on ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1 preparation solution

[0051] Mixed standard stock solution: pipette 2mL multi-element mixed standard solution (GBW08607: Pb concentration is 1.03μg / g, Cd concentration is 0.104μg / g, Cr concentration is 0.516μg / g). Dissolve in 25mL of deionized water and shake well to obtain a mixed standard stock solution with a Pb concentration of 82.4 μg / L, a Cd concentration of 8.32 μg / L, and a Cr concentration of 41.28 μg / L.

Embodiment 2

[0052] Example 2 Using ionic liquid and nitric acid to sample pretreatment

[0053] HNO 3 It is a commonly used solvent when digesting samples. The wet digestion of food solid samples usually requires 14mL concentrated nitric acid and 1mL perchloric acid. The temperature is between 200°C and 300°C. into the environment. The sample selected in this embodiment is dried fungus, concentrated HNO 3 The dosage is 0.5mL. The applicant found through experiments that when the heating temperature is higher than 200°C, the sample will be carbonized in the ionic liquid [Bmim]-Cl solution, so the heating temperature selected in this embodiment is 170°C, and the reaction will be free of solid particles in the solution, and the solution will be The light-colored and bright shape is considered to be completely dissolved, and the dissolution status is shown in Table 4.

[0054] The dissolving time of table 4 food solid sample

[0055]

[0056] It can be seen from Table 4 that the solut...

Embodiment 3

[0057] Example 3 Pretreatment of Food Solid Samples Based on Ionic Liquids

[0058] Accurately weigh 3g of ionic liquid [Bmim]-Cl and place it in a beaker, heat the beaker to 90°C to melt the ionic liquid [Bmim]-Cl crystals, remove and cool after completely melting, and accurately weigh 0.2g of sample powder into the beaker , the sample was evenly dispersed on the liquid surface, and 0.5mL concentrated HNO was added 3 , heated to 160°C, and dissolved for 5 minutes. After it dissolves, add deionized water to precipitate the cellulose, and set the volume to 50mL. After the precipitated cellulose settles naturally, take part of the upper clear night, and use graphite furnace atomic absorption spectrometry to detect it. The results are shown in Table 5. Show.

[0059] Table 5 Analysis result samples after pretreatment

[0060]

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Abstract

The invention provides a pretreatment method for a solid food sample based on ionic liquid, and the method comprises the following steps: contacting the ionic liquid with a to-be-treated solid food sample, performing heating under the condition of concentrated HNO3 until the sample is completely dissolved, adding deionized water, and performing filtering. Compared with wet digestion, the pretreatment method established by the invention has the advantages that the pretreatment time can be shortened by 36-48 times, and the dosage of the acid liquor is reduced by 12-20 times, so that a green, safe and rapid pretreatment technology in heavy metal ion detection and analysis of the food solid sample is provided.

Description

technical field [0001] The invention relates to the field of detection and analysis of heavy metal ions, in particular, the invention relates to a pretreatment method based on ionic liquids. Background technique [0002] Due to the complex composition of food samples, especially solid food samples, the low content of heavy metal ions, and the diversity of valence and form in some heavy metal elements, the detection and analysis of heavy metal ions in food samples (especially solid food samples) Before, the sample must be properly pre-treated. [0003] For the pretreatment technology for the detection and analysis of heavy metal ions in solid food samples, the commonly used methods are ash method, microwave digestion method or acid digestion method, among which microwave digestion method and acid digestion method are the most commonly used. These methods generally use strong acid and strong oxidizing reagents to decompose the sample under high temperature and high pressure c...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/44G01N1/38G01N1/34G01N21/31
CPCG01N1/28G01N1/44G01N1/38G01N1/34G01N21/3103Y02P20/54
Inventor 凌约涛王遥雪张霖潘瑞花王帆郭少飞
Owner 武汉海关技术中心
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