Method used for detecting 2,4-dichlorophenoxyacetic acid residue in fruits and vegetables

A dichlorophenoxyacetic acid and detection method technology, which is applied in the direction of measuring devices, instruments, and material analysis through optical means, can solve the problems of cumbersome operation, low analysis sensitivity, and inappropriate on-site detection and analysis of a large number of samples

Inactive Publication Date: 2017-08-15
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2,4-D is difficult to degrade in nature, so 2,4-D is easy to leach and migrate into water and soil, and then accumulate in organisms, which is harmful to human health and natural ecological environment
Because it contains a strong polar carboxyl group, the chromatographic peaks are tailed when the first two methods are directly detected, and the analysis sensitivity is low. In order to improve the volatility of the weak acid, it needs to be derivatized into an ester before detection
The introduction of derivatization makes the operation cumbersome and time-consuming
Liquid chromatography analysis does not require derivatization, but the pretreatment and purification requirements are strict and the operation is cumbersome, so it is not suitable for on-site detection and analysis of a large number of samples

Method used

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  • Method used for detecting 2,4-dichlorophenoxyacetic acid residue in fruits and vegetables
  • Method used for detecting 2,4-dichlorophenoxyacetic acid residue in fruits and vegetables
  • Method used for detecting 2,4-dichlorophenoxyacetic acid residue in fruits and vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Configure 2,4-D methanol aqueous solution with a concentration of 20, 15, 10, 5, 2, 1 μg / mL, mix it with the gold colloid in step 1 at a ratio of 1:5, and scan the Raman spectrum to obtain the concentration gradients Surface-enhanced Raman spectrum of the solution; 2,4-D characteristic peaks are 718, 838, 890, 1159, 1256, 1308, 1445, 1591cm -1 ; and take the concentration as the abscissa, and take the characteristic peak 838cm -1 The peak intensity is the ordinate, and a standard curve is made for quantification; such as figure 1 , figure 2 As shown, the linear equation of the standard curve obtained is y=(13.6±0.66)x+(176.0±7.39), the correlation coefficient is 0.9907, and the linearity is good, which can be used to determine the 2,4-D content in the sample.

Embodiment 2

[0029] Accurately weigh 10.0g of the vegetable sample, fully break the sample with a sample masher or a homogenizer, then put the mashed vegetables into a centrifuge tube, add 10mL of 0.01mol / L NaOH solution, shake and extract for 2-10min, 8000r Centrifuge at a speed of 5 min / min, take the supernatant, then add NaOH solution, shake and extract for 2-10 min, repeat the above operation, combine the extracts, adjust the pH to 3.0 with 1mol / L hydrochloric acid, pass through a 0.45um filter membrane, and extract all The liquid passes through the activated solid-phase extraction column at a flow rate of 3mL / min. After the sample is loaded, it is rinsed with 3mL aqueous hydrochloric acid solution. 3 OH elution, repeated 4 times, combined eluent, blown to near dryness with nitrogen, fixed solution with methanol aqueous solution to 2mL, used for surface-enhanced Raman spectrum detection, made three parallel samples, and the analysis results are shown in Table 1; It can be seen that the...

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Abstract

The invention discloses a method used for rapidly detecting 2,4-dichlorophenoxyacetic acid (2,4-D) residue in fruits and vegetables via surface enhanced Raman spectroscopy (SERS). According to the method, gold sol is prepared via reduction of chloroauric acid with trisodium citrate; a 2,4-D-containing solution to be detected is mixed with gold sol; a portable Raman spectrometer is adopted for Raman spectrum scanning so as to obtain the surface enhanced Raman spectrum of 2,4-D; the characteristic peaks of 2,4-D can be observed at 1159cm<-1>, 838 cm<-1>, 890 cm<-1>, 718 cm<-1>, 1256 cm<-1>, 1308 cm<-1>, 1445 cm<-1>, and 1591 cm<-1>, and the peak strength of the characteristic peak at 838 cm<-1> is used for quantitative determination of the content of 2,4-D. According to the method, SERS is adopted to develop the method used for rapid, accurate, portable, and simple detection of 2,4-D residue, and the method is suitable for food safety on-site real-time rapid screening.

Description

technical field [0001] The invention belongs to the field of food safety monitoring, and in particular relates to a detection method for 2,4-dichlorophenoxyacetic acid residues in fruits and vegetables. Background technique [0002] 2,4-Dichlorophenoxyacetic acid (2,4-D) is a low-toxicity pesticide according to my country's pesticide toxicity classification standards, and has been registered in some vegetables and grains in my country. 2,4-D has strong biological activity on plants, and is a kind of efficient, systemic and highly selective herbicide and plant growth regulator. At high concentration, 2,4-D is a broad-spectrum herbicide, which is widely used in grass crops such as rice, corn, wheat, broad-leaved weeds in lawns and pastures; at low concentration, 2,4-D acts as Plant growth regulators can promote crop growth, increase fruit setting rate, increase fruit size, etc. In addition, as a food additive, 2,4-D is also a widely used fruit antiseptic and preservative, mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 张萍郑大威曹智王惠琴林太凤易鹏刘晓莹卫晓丹
Owner BEIJING UNIV OF TECH
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