Method for detecting content of carbaryl in food by combining liquid phase micro-extraction with thread microfluid colorimetry
A colorimetric, carboxylate technology, which is used in measuring devices, material analysis, instruments, etc. by observing the effect on chemical indicators, to achieve the effect of simple and fast operation process, less sample required, and rapid detection.
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Embodiment 1
[0066] Embodiment 1, cotton thread pretreatment
[0067] Put the cotton thread in 10mg mL -1 Na 2 CO 3 Wash in boiling solution for 5min. Then, the cotton thread is rinsed with distilled water until the pH of the rinse solution is neutral, dried at room temperature and stored in a desiccator for future use.
Embodiment 2
[0068] Embodiment 2, effervescence-assisted liquid phase microextraction condition optimization based on convertible solvent solidification
[0069] A. Types of extractants
[0070] (1) Experimental method: Weigh 1 g of crushed sample, add 100 μL of carbaryl (10 mmol L -1 , methanol) and 1 mL of acetonitrile solution, vortex extraction for 3 min. Filter the extract with a membrane (0.22 μm), take 600 μL sample filtrate and add 4.4 mL water to a 10 mL centrifuge tube. Add 40 mg of sodium carbonate to adjust the pH of the solution to alkaline so that carbaryl is hydrolyzed into 1-naphthol, add 80 μL of hydrophobic extractant (caprylic acid, nonanoic acid, capric acid), and the extractant is converted into water-soluble Ionic form, dispersed in the sample solution. Then 70 mg of citric acid was added to generate an extractant in situ for extraction, and the bubbles generated by the effervescent reaction resulted in a larger surface area between the extraction solvent and the a...
Embodiment 3
[0090] Embodiment 3, partial optimization of thread microfluidic detection
[0091] a. Adjust the pH of the solution for optimization
[0092] (1) Experimental method: Cut the treated cotton thread into small pieces with a length of 1±0.1cm, and paste them on a white plastic board with double-sided adhesive tape. Prepare aqueous solutions of different pH (pH=1, pH=2, pH=3, pH=4, pH=5, pH=6, pH=7, pH=8, pH=9, pH=10, pH=11, pH=12, pH=13, pH=14, the pH is adjusted with HCl in the range of 1-6, and the pH is adjusted with NaOH in the range of 7-14). First add 5 μL of aqueous solutions of different pH to a 1 cm cotton thread, after the thread is wet, add 5 μL of 4-methoxybenzenediazotetrafluoroborate (10 mmol L -1 ), dry at room temperature, and finally add 7 μL 1-naphthol octanoic acid solution (concentration is 1mmol L -1 ), after 20 minutes of reaction, take pictures and calculate the RGB intensity (I).
[0093] (2) The experimental results are as follows Figure 9 shown. ...
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