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Application method for detecting hormone in food by joint SERS (Surface Enhanced Raman Scattering) substrate

An application method and substrate technology, applied in the fields of nanomaterials, food safety testing, and photonic materials, can solve problems such as long half-life, difficult biodegradation, and hormone residues, and achieve the effects of low detection limit, high sensitivity, and high sample recovery rate

Active Publication Date: 2017-10-24
ACADEMY OF MILITARY MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After entering the body, hormones accumulate for a long time, have a long half-life, and are difficult to biodegrade, leading to increasingly serious problems of hormone residues

Method used

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  • Application method for detecting hormone in food by joint SERS (Surface Enhanced Raman Scattering) substrate
  • Application method for detecting hormone in food by joint SERS (Surface Enhanced Raman Scattering) substrate
  • Application method for detecting hormone in food by joint SERS (Surface Enhanced Raman Scattering) substrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Uniformity, repeatability and stability investigation of a combined SERS substrate:

[0033] figure 1 The given Fe3O4@SiO2-Ag-C6+ rod silver SERS signal quality research map. From figure 1 a It can be seen that the 15 SERS curves are basically the same, and the Raman characteristic peak of diethylstilbestrol is 1028cm -1 As a reference, the calculated relative standard deviation of the Raman peak intensities of 15 SERS spectra is 4.88%, indicating that the substrate has good uniformity. Day-to-day repeatability, 25 Raman spectrum peaks are obtained, intra-day repeatability is 15 Raman spectrum peaks, batch repeatability, a total of 15 Raman spectrum peaks are collected three times, such as figure 1 b, c, d, at 1028cm -1The histograms of the intensity values ​​of the SERS signal at the position are shown in b, c, and d illustrations, respectively. The acquired SERS spectra show good uniformity, and the dispersion of the SERS signal intensity is relatively large. The...

Embodiment 2

[0035] The application method of using SERS substrate to detect hormones in food is used for qualitative and quantitative analysis of two hormone solutions:

[0036] figure 2 It is the qualitative and quantitative analysis result of diethylstilbestrol solution. We have a concentration range of 10 -5 ~10 -12 The diethylstilbestrol solution of M is detected by Raman, and the 80% methanol of the diethylstilbestrol solution is used as a signal reference, and the obtained SERS spectrum is as follows figure 2 As shown in A. Such as figure 2 As shown in a, we choose 1028cm -1 The log-log curve has been drawn as the characteristic peak of diethylstilbestrol, and the standard deviation of the measurement result is presented in the figure in the form of error bars, at 10 -5 ~10 -12 Within the concentration range of M, the obtained linear equation is y=12661+8044.1465x, r 2 =0.97, the linear relationship is good. The detection limit of this method for diethylstilbestrol is 5p...

Embodiment 3

[0039] Figure 4-Figure 6 It is the qualitative and quantitative analysis results of diethylstilbestrol in milk and 17β-estradiol in milk. Taking blank milk as a signal reference, the obtained SERS spectrum is as follows: Figure 4 A. Figure 5 Shown in B. Such as Figure 4 a, Figure 5 As shown in b, we selected the characteristic peaks of diethylstilbestrol and 17β-estradiol in the spectrum at 1028cm -1 and 1449cm -1 , draw log-log curves according to their corresponding concentrations in solution. As the concentration of hormones decreased, their intensity corresponding to the characteristic peaks in the SERS spectrum also gradually decreased, diethylstilbestrol and 17β-estradiol were respectively -3 ~10 -10 M and 10 -3 ~10 -8 Within the concentration range of M, the linear equations are y=40532+3495.8084x, r 2 =0.99; y=35161+3540.0586x, r 2 = 0.99, all linear relationships are good. The detection limits of diethylstilbestrol and 17β-estradiol in milk by this m...

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Abstract

The invention discloses an application method for detecting a hormone in food by a joint SERS (Surface Enhanced Raman Scattering) substrate. A detection method comprises the following steps of firstly preparing n-hexanethiol modified magnetic nano silver flower; secondly, using diethylstilbestrol as an experimental subject, and investigating and researching the homogeneity, the repetitiveness and the stability of the joint SERS substrate of a Fe3O4@SiO2-Ag-C6+ sliver rod; diluting two hormones to have different concentrations respectively by using methanol water and milk, and purifying and enriching by using a SPE (Solid Phase Extraction) column; adding eluant to the SERS substrate respectively, drying, then dotting on the silver rod, carrying out raman spectrum detection, and determining a lowest detection limit. The standard addition recovery rate is 88.72 percent to 110.04 percent; the application method has a relatively high recovery rate; the requirement on the analysis of a residue of the hormone in the food can be completely met. The invention also discloses the joint SERS substrate of the Fe3O4@SiO2-Ag-C6+ silver rod, which is prepared by the method. The joint SERS substrate has abundant hotspots, and can be used for making up the loss, which is brought as C6 is adsorbed on the surface of a silver crust, of a raman signal.

Description

technical field [0001] The invention relates to the research on the uniformity, repeatability and stability of SERS signals combined with a SERS substrate, in particular to an application method for detecting hormones in food with a combined SERS substrate, belonging to the fields of photonic materials, nanomaterials, and food safety detection. Background technique [0002] Hormones are widely distributed in nature and are a class of steroid hormones with similar chemical structures. They are divided into endogenous estrogens and exogenous estrogens. One end of them contains a long aliphatic hydrocarbon chain with a carboxyl group, which can directly affect Animal metabolism and reproduction. After entering the body, hormones accumulate for a long time, have a long half-life, and are difficult to biodegrade, leading to increasingly serious problems of hormone residues. There are many ways for humans to consume hormones, among which dairy products are the main source. Childr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 王升启李萍肖瑞汪崇文李敏荣振
Owner ACADEMY OF MILITARY MEDICAL SCI
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