A kind of electrochemical rapid detection method of semicarbazide
A detection method and electrochemical technology, applied in the field of analytical chemistry, can solve the problems of high detection cost of equipment, unsuitable to carry, death of rats, etc., and achieve the effect of low detection cost, small detection tools and high sensitivity of the method
Active Publication Date: 2019-11-15
SOUTH CHINA UNIV OF TECH
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Problems solved by technology
As for semicarbazide, injecting 40mg / kg semicarbazide to juvenile rats will have a huge impact on the secretion level of sex hormones and multiple reproductive organs in rats, and continuing to increase the intake will lead to the death of rats
[0003] There are existing detection methods for semicarbazides such as high performance liquid chromatography coupled with ultraviolet and fluorescence detectors, liquid chromatography mass spectrometry, etc., but these equipments are expensive to detect and are not suitable for carrying, and this high-performance technology is widely used in applications subject to certain restrictions
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[0024] This embodiment carries out the detection of semicarbazide content to 6 different types of flour products on the market:
[0025] (1) Pretreatment of samples to be tested:
[0026] Weigh 1.0000g (accurate to 0.0001g) of noodle products and dissolve them in 10mL of 0.2mol / L hydrochloric acid solution, mix well with a vortex mixer and then perform ultrasonic treatment, then add 1mL of 0.1mol / L o-nitrobenzaldehyde (o-nitrobenzaldehyde The benzaldehyde solution was prepared with methanol and stored in a dark place below 4°C, and its shelf life was one week), and then reacted at 37°C for 16 hours after mixing on a vortex mixer. After the reaction, cool to room temperature, centrifuge, take the supernatant, adjust the pH between 6 and 7 with 0.2mol / L hydrochloric acid and 0.3mol / L potassium phosphate solution, then extract with 5mL ethyl acetate, take the organic phase Blow dry with nitrogen at room temperature to remove ethyl acetate, dissolve the obtained extract in 5 mL o...
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Abstract
The invention belongs to the technical field of analytical chemistry, and discloses an electrochemical quick detecting method of semicarbazide. The electrochemical quick detecting method comprises the following steps: adding a to-be-detected sample into a hydrochloric acid solution, adding a derivating agent for carrying out semicarbazide derivatization reaction, centrifuging a reaction solution, taking supernatant, extracting by using an organic solvent after regulating a pH (Potential of Hydrogen) value to be 6 to 7, taking and blow-drying an organic phase by using nitrogen gas, removing the organic solvent, and filtering by using a filter membrane after dissolving an extract in a base solution, thus obtaining a pretreated to-be-detected sample; respectively preparing semicarbazide standard solutions in different concentrations, measuring electrochemical signals in sample solutions in different concentrations by adopting a portable electrochemical working station, and drawing a standard curve; then testing electrochemical signals in the to-be-detected sample, and calculating through the standard curve, thus obtaining the concentration of the semicarbazide in the to-be-detected sample. The electrochemical quick detecting method disclosed by the invention is high in sensitivity and low in detection cost, and is capable of realizing on-site quick detection on the semicarbazide.
Description
technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to an electrochemical rapid detection method of semicarbazide. Background technique [0002] Semicarbazide, is a white crystal, easily soluble in water, the chemical formula is H 2 N-NH-CO-NH 2 . It is a metabolite of azodicarbonamide, a noodle product additive. Many countries in the world, such as Canada, the European Union and the United States, stipulate that the dosage of azodicarbonamide should be less than 45mg / kg. Unsupervised [2009] No. 89) and Ministry of Health Announcement No. 6 in 2011, etc., in the 2011 Food Additive Product Standard Announcement (Ministry of Health Announcement No. 8 in 2011) the maximum amount of azodicarbonamide used in wheat flour is 0.045g / kg (GB2760-2007). As for semicarbazide, injecting 40mg / kg semicarbazide to juvenile rats will have a huge impact on the secretion level of sex hormones and multiple reproductive orga...
Claims
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IPC IPC(8): G01N27/48
CPCG01N27/48
Inventor 朱玉丹杭义萍
Owner SOUTH CHINA UNIV OF TECH