Method for detecting sodium thiocyanate in milk based on mof sERS technology

A technology of sodium thiocyanate and technical detection, applied in the field of analysis and detection, to achieve the effects of simple pretreatment method and detection operation, improved capture ability, and improved surface plasmon resonance performance

Active Publication Date: 2022-08-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, MOFs materials are mainly used in chemical industry, biology and other fields, but because of their large pore volume, high surface area, excellent adsorption performance and high chemical stability, they are also gradually tried to be used as SERS substrates. However, there are few reports on the actual application direction of SERS detection

Method used

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  • Method for detecting sodium thiocyanate in milk based on mof sERS technology
  • Method for detecting sodium thiocyanate in milk based on mof sERS technology
  • Method for detecting sodium thiocyanate in milk based on mof sERS technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Preparation of Example 1 Substrate

[0053] The preparation method of nano-silver SERS substrate grown on the surface of MIL-101(Fe) material includes the following steps:

[0054] (1) Synthesis of MIL-101(Fe) material:

[0055] Weigh 0.675g of ferric chloride hexahydrate and 0.206g of terephthalic acid, add in 15mL of dimethylformamide, stir and dissolve to obtain a mixed solution; then transfer the mixed solution to a tetrafluoroethylene-lined heating kettle, It was placed in a muffle furnace, heated and reacted at 150°C for 6 hours, and cooled to room temperature to obtain an orange-yellow product; the product was centrifuged at 10,000 rpm for 10 minutes to collect the precipitate, and the obtained orange-yellow solid precipitate was treated with dimethylformamide and Wash three times each with absolute ethanol, and dry at 70°C for 3 hours to obtain an orange solid powder, namely MIL-101(Fe) material powder;

[0056] (2) preparation concentration is the silver nitr...

Embodiment 2

[0060] Construction of Example 2 Model

[0061] The construction method of the linear model of the characteristic peak intensity of sodium thiocyanate and the concentration of sodium thiocyanate includes the following steps:

[0062] (1) Prepare the mother liquor of sodium thiocyanate with a concentration of 1g / L, then take the mother liquor and dilute to 1, 2, 3, 4, 5, 6, 8, 10, 12.5, 15, 20, 25, 30, 40, 50mg respectively. / L standard solution of sodium thiocyanate;

[0063] (2) The standard solutions of sodium thiocyanate of different concentrations and milk are mixed uniformly according to the volume ratio of 1:9 to form milk sample solutions of different concentrations of sodium thiocyanate;

[0064] (3) according to the milk sample liquid and ethanol according to the volume ratio of 1:1 mix evenly, centrifuge to obtain the supernatant of different sodium thiocyanate concentration;

[0065] (4) The supernatant and the nano-silver SERS substrate grown on the surface of th...

Embodiment 3

[0070] A method for detecting sodium thiocyanate in milk based on surface-enhanced Raman technology (such as Figure 4 ), including the following steps:

[0071] (1) the milk with the sodium thiocyanate concentration of 0.5, 1, and 1.5 mg / L is mixed with absolute ethanol according to the volume ratio of 1:1, and centrifuged to obtain a supernatant;

[0072] (2) The supernatant and the nano-silver SERS substrate grown on the surface of the MIL-101(Fe) material prepared in Example 1 were uniformly mixed according to a volume ratio of 1:1, and allowed to stand for 4 minutes to conduct Raman detection to obtain the Raman spectrum (eg Figure 5 );

[0073] (3) Set the Raman spectrum obtained in step (2) at 2110 cm -1 ±5cm -1 The intensity of the characteristic peak of sodium thiocyanate is substituted into the linear model of the intensity of characteristic peak of sodium thiocyanate and the concentration of sodium thiocyanate in Example 2 to obtain the concentration of sodium ...

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Abstract

The invention discloses a method for detecting sodium thiocyanate in milk based on the SERS technology of MOF, and belongs to the field of analysis and detection. The method of the present invention comprises the following steps: (1) growing nano-silver on the surface of MIL-101(Fe) material to obtain a nano-silver SERS substrate grown on the surface of MIL-101(Fe) material; (2) growing the milk to be tested After pretreatment with absolute ethanol, the supernatant is obtained by centrifugation, and then the supernatant and the SERS substrate obtained in step (1) are mixed uniformly, and Raman detection is performed to obtain a Raman spectrum; Raman spectrum at 2110cm ‑1 ±5cm ‑1 The characteristic peak intensity of sodium thiocyanate at 1 is substituted into the linear model of the characteristic peak intensity of sodium thiocyanate and the concentration of sodium thiocyanate to obtain the concentration of sodium thiocyanate in the milk to be tested. The detection limit of the method of the invention is as low as 96.3 μg / L, the recovery rate is 97.03%-106.46%, has good detection accuracy, and is of great significance for supervising the illegal addition of sodium thiocyanate in milk.

Description

technical field [0001] The invention relates to a method for detecting sodium thiocyanate in milk based on MOF-based SERS technology, and belongs to the field of analysis and detection. Background technique [0002] Sodium thiocyanate is a chemical raw material widely used in medicine, chemistry, printing and other fields. At the same time, due to its good natural antibacterial effect and low price, it is used as a common preservative in the food industry. In recent years, some illegal traders choose to add excessive sodium thiocyanate to milk in order to reduce the cost of milk sterilization and cover up the inferior quality of milk. However, studies have shown that excessive sodium thiocyanate will hinder the body's absorption of iodine and affect thyroid hormones. The production of iodine and the metabolism of iodine can easily lead to goiter, which is harmful to human health. [0003] At present, the main methods for the detection of sodium thiocyanate in milk are: spec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65G01N1/28
CPCG01N21/658G01N1/28
Inventor 陈国庆王子睿吴亚敏马超群李磊朱纯高辉辜姣
Owner JIANGNAN UNIV
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