Sample pretreatment method suitable for detection of basic orange II in bean product

A sample pretreatment and basic orange technology, applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of large amount of organic solvent, long sample processing time, low sample detection efficiency, etc., and achieve short processing time , protection of the environment and the health of the analyst, high selectivity and efficient enrichment and purification effects

Inactive Publication Date: 2015-08-12
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current national standard method (GB / T 23496-2009) uses the traditional liquid-liquid extraction (Liquid-Liquid Extraction, LLE) for sample pretreatment of Basic Orange II in soybean products. The time is long, which is not conducive to environmental protection, and the sample detection efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Sample: Yuba.

[0026] Target substance: Basic Orange II.

[0027] Nylon 6 was used as a raw material, and a mixed solution of m-cresol and formic acid (4:6, v / v) was used as a solvent, and stirred and mixed at room temperature for 12 hours to obtain a nylon 6 solution with a concentration of 25 wt%. Using electrospinning method, at 30% humidity, 20°C temperature, and 15kV voltage, the syringe is advanced at a speed of 0.2mL / h, the distance between the injection needle tip and the receiving device is 15cm, electrospinning for 2 hours, and the film thickness is collected Nylon 6 nanofiber membrane with a fiber diameter of about 70 μm and a fiber diameter of about 200 nm.

[0028] Weigh 1.0g of bean curd stick powder, add 1mL of ethanol to homogenize, then add 10mL of extract---ammonia water to adjust the pH to 8 in 60% ethanol aqueous solution (ethanol:water=70:30, v / v), vortex mix At room temperature, ultrasonically extract for 30 min, centrifuge at 10,000 r / min for 5...

Embodiment 2

[0031] Sample: fried tofu.

[0032] Target substance: Basic Orange II.

[0033] Using nylon 6 as raw material and a mixed solution of m-cresol and formic acid (4:6, v / v) as solvent, stir and mix at room temperature for 8 hours to obtain a nylon 6 solution with a concentration of 32 wt%. Using the electrospinning method, at a humidity of 30%, a temperature of 20°C, and a voltage of 18kV, the syringe is advanced at a speed of 0.5mL / h, the distance between the injection needle tip and the receiving device is 20cm, electrospinning for 4 hours, and the film thickness is collected Nylon 6 nanofiber membrane with a fiber diameter of about 120 μm and a fiber diameter of about 230 nm.

[0034]Weigh 2.0g of oily tofu, crush it, add 1mL of ethanol to homogenize, add 5mL of n-hexane, vortex for 30s, ultrasonic for 30min, centrifuge for 5min, discard the n-hexane layer, then add 10mL of extract solution---hydrogenation 80% ethanol aqueous solution (ethanol:water=70:30, v / v) with sodium a...

Embodiment 3

[0037] Sample: soy milk.

[0038] Target substance: Basic Orange II.

[0039] Nylon 6 was used as a raw material, and a mixed solution of m-cresol and formic acid (4:6, v / v) was used as a solvent, and stirred and mixed at room temperature for 15 hours to obtain a nylon 6 solution with a concentration of 30 wt%. Using electrospinning method, at 30% humidity, 20°C temperature, and 16kV voltage, the syringe is advanced at a speed of 0.1mL / h, the distance between the injection needle tip and the receiving device is 25cm, electrospinning for 2 hours, and the film thickness is collected Nylon 6 nanofiber membrane with a fiber diameter of about 80 μm and a fiber diameter of about 180 nm.

[0040] Weigh 1.0g of soymilk powder, add 1mL of ethanol to homogenize, add 10mL of extract --- 70% ethanol aqueous solution (ethanol:water=70:30, v / v) with ammonia water to adjust the pH to 12, and vortex to mix At room temperature, ultrasonically extract for 30 minutes, centrifuge at 10,000 r / mi...

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Abstract

The invention provides a sample pretreatment method for detecting basic orange II in a bean product based on a nylon 6 nanometer fiber membrane. The method comprises: 1) preparing a nylon 6 nanometer fiber membrane, wherein the nylon 6 nanometer fiber membrane is prepared by using an electrospinning solution through an electrostatic spinning method; and 2) extracting and purifying the basic orange II in a bean product sample, wherein the nylon 6 nanometer fiber membrane is made into a round sheet with a diameter of about 10-60 mm, the round sheet is arranged on a membrane disk type solid phase extraction instrument, the basic orange II is adsorbed on the nylon 6 nanometer fiber membrane, the obtained nylon 6 nanometer fiber membrane is leached with a washing agent so as to remove the impurity possible of being subjected to adsorption with the basic orange II molecules, and the basic orange II is eluted from the nylon 6 nanometer fiber membrane with an eluant so as to carry out analysis detection. According to the present invention, the high selectivity and high-efficiency enrichment and purification can be performed on the basic orange II dye in various actual bean product samples only with several milligrams of the nylon 6 nanometer fiber membrane and several hundred microliters of the eluant, wherein the sample matrix does not affect the detection on the target product, and the extraction efficiency is substantially improved compared with the commercially-produced solid-phase extraction small column.

Description

technical field [0001] The invention provides a sample pretreatment method suitable for the detection of basic orange II in soybean products. The invention belongs to the technical field of sample pretreatment in analytical chemistry. Background technique [0002] Basic orange Ⅱ (Chrysoidine), commonly known as king golden yellow, block yellow, is an azo industrial dye, mainly used in the dyeing of textiles, leather products and wood products. Because of its good coloring and low price, it is illegally added to foods such as soybean products, aquatic products, and condiments. At present, conclusive animal experiment data have shown that this substance is a carcinogen. Therefore, it will bring great health hazards after being ingested into the human body through food. This substance is one of the first batch of non-edible pigments included in the list of "non-edible substances that may be illegally added in food" by the Ministry of Health of my country. Therefore, it is v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N30/06
Inventor 许茜祁菲菲李晓晴
Owner SOUTHEAST UNIV
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