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Method for rapidly detecting paraquat by utilizing Raman spectrometry

A technology of Raman spectroscopy and paraquat, which is applied in Raman scattering, measuring devices, and material analysis through optical means, and can solve problems such as cumbersome, photochemical reaction interference detection, and detection interference.

Inactive Publication Date: 2017-05-31
南京简智仪器设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is reported in the literature that Zou Mingqiang et al. established a laser Raman spectroscopy method for the rapid determination of trace amounts of paraquat in fruits and vegetables. The detection limit is low and portable detection is realized. However, it is difficult to avoid redundant The photochemical reaction caused by grease and other substances interferes with the detection. At the same time, the method needs to mix the silver colloid solution with the solution containing chloride ions in advance to form a detection reagent, which is relatively cumbersome, and the chlorine-induced photochemical reaction interferes with the detection.

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  • Method for rapidly detecting paraquat by utilizing Raman spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1. Determination of the content of paraquat in wastewater. details as follows.

[0017] (1) Prepare paraquat standard solution: Accurately weigh 0.010 g of paraquat standard product, dissolve it in water, dilute it to 100 mL, store it in the dark at 4 ℃, and dilute the standard solution to 5 μg / kg, 50 μg / kg, and 250 μg respectively / kg, 500μg / kg, 1000μg / kg, 2000μg / kg series of standard solutions for use.

[0018] (2) Preparation of the sample solution to be tested: take 2mL of waste water and filter it with a 0.45μm microporous membrane.

[0019] (3) Draw a standard curve and measure samples: set the laser power of the Raman spectrometer with a wavelength of 785 nm to 100 mW, an integration time of 1 s, an average of 2 times, a smoothing parameter of 5, and a scanning range of 300 to 4500 cm -1 . For each standard solution, add 1 volume of silver nanoparticle sol and 4 volumes of standard solution to a 1 cm optical glass cuvette quickly and sequentially withi...

Embodiment 2

[0020] Example 2. Determination of whether paraquat is contained in wastewater is as follows.

[0021] (1) Preparation of the sample solution to be tested: Take 2 mL of wastewater and filter it with a 0.45 μm microporous membrane.

[0022] (2) Set the wavelength of the Raman spectrometer to 785 nm, the laser power of the laser is 100 mW, the integration time is 1 s, the average times is 1 time, the smoothing parameter is 5, and the scanning range is 300~4500 cm -1 . Add 1 volume of silver nanoparticle sol and 4 volumes of standard solution to a 1 cm optical glass cuvette quickly and sequentially within 10 s, and place them in the detection chamber of a laser Raman spectrometer for detection. After testing, at 1193, 1292, 1648 cm -1 ±3cm -1 A characteristic peak appears at the position, indicating that the water body to be tested contains paraquat.

Embodiment 3

[0023] Example 3. Determination of the content of paraquat in tomatoes. details as follows.

[0024] (1) Prepare paraquat standard solution: Accurately weigh 0.010 g of paraquat standard product, dissolve it in water, dilute it to 100 mL, store it in the dark at 4 ℃, and dilute the standard solution to 5 μg / kg, 50 μg / kg, and 250 μg respectively / kg, 500μg / kg, 1000μg / kg, 2000μg / kg series of standard solutions for use.

[0025] (2) Preparation of sample solution to be tested: Weigh 2g of tomato sample and 2mL of water, shake and mix, centrifuge at 8000 rpm for 5 minutes, take the supernatant, and filter to obtain the solution to be tested.

[0026] (3) Draw a standard curve and measure samples: set the laser power of the Raman spectrometer with a wavelength of 785 nm to 100 mW, an integration time of 1 s, an average of 2 times, a smoothing parameter of 5, and a scanning range of 300 to 4500 cm -1 . For each standard solution, add 1 volume of silver nanoparticle sol and 4 volu...

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Abstract

The invention relates to a method for rapidly detecting paraquat by utilizing Raman spectrometry and in particular relates to application to rapid detection of environments and foods. Specifically, the method comprises the following steps: taking silver nano-sol as a Raman detection enhancing agent; mixing one volume of the silver nano-sol with four volumes of a solution to be detected; rapidly determining a Raman signal under low power; realizing qualitative and quantitative detection on the paraquat according to preferable characteristic peak positions and strength. Photochemical reaction is effectively avoided under preferable testing conditions of low-power laser effect and no chlorine addition, so that the content of the residual paraquat in actual environment water bodies and foods is rapidly, accurately and conveniently determined; meanwhile, incorrect measurement is effectively avoided through a preferable characteristic peak combination; the method is especially suitable for being matched with a realization scene of a handheld Raman analyzer and outdoor real-time analysis.

Description

technical field [0001] The invention belongs to the field of analysis and detection of substances, in particular to the technical field of rapid detection of environment and food safety. Background technique [0002] Paraquat (PQ) also known as paraquat, Gramoxone, 1,1’-dimethyl-4,4’-bipyridine cationic salt, molecular formula: C 12 h 14 Cl 2 N 2 , Molecular weight 257.2, CAS No.: 1912-24-9, is an organic heterocyclic contact defoliant and herbicide with a solubility of 700 g / L (20°C), easily soluble in water. Paraquat can be quickly absorbed by the green tissue of plants, causing them to die. It is currently widely used on more than 50 crops in more than 120 countries around the world. However, long-term ingestion, inhalation or skin contact with paraquat can cause kidney, liver and heart problems, resulting in spots in the lungs and narrowing of the esophagus. In addition, it also has obvious irritating effects on the skin and mucous membranes, which can cause serious...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 殷磊蔡圣闻夏静竹
Owner 南京简智仪器设备有限公司
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