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Method for quickly detecting aflatoxin B1 content in traditional Chinese medicinal materials

A technology of aflatoxin and Chinese medicinal materials, applied in the field of analysis and testing, can solve the problems of complex detection process, high detection limit, unstable enzyme, etc., and achieve the effect of simplifying the experimental process, saving drugs and saving time

Inactive Publication Date: 2016-08-17
ZHAOQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the sensitivity of liquid chromatography cannot reach the required range, the detection limit is high, and the detection process of fluorescence detection is complicated
ELISA detection is fast, but due to the extremely unstable enzymes used, the false positive rate is relatively high, which has a significant impact on both qualitative and quantitative

Method used

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  • Method for quickly detecting aflatoxin B1 content in traditional Chinese medicinal materials
  • Method for quickly detecting aflatoxin B1 content in traditional Chinese medicinal materials
  • Method for quickly detecting aflatoxin B1 content in traditional Chinese medicinal materials

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Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: the method for rapid determination of aflatoxin B1 content in Chinese medicinal materials of the present invention

[0024] The rapid determination method of the present invention is applicable to the rapid detection of aflatoxin B1 content in Chinese herbal medicine samples, and the method comprises the following steps:

[0025] (1) QuEChERS extraction: Take 5.00g of Chinese herbal medicine samples, pulverize and grind to obtain a sample powder with a particle size of 0.02mm, add it to a 100mL conical flask; prepare 50mL of acetonitrile-water (volume ratio: 90:10) solution in the volumetric flask , added to the Erlenmeyer flask, shaken at 350r / min for 25min, left to settle, filtered, and the supernatant was taken through a purification column, concentrated and passed through a 0.22μm filter membrane to be tested;

[0026] (2) Adopt ultra-high performance liquid chromatography-triple quadrupole mass spectrometry to detect the liquid to be tested;

[0027]...

Embodiment 2

[0032] Embodiment 2: the improvement of QuEChERS extraction method

[0033] Take the sample and grind it to get 5.00g of powder with a particle size of 0.02mm, add it to a 100mL conical flask, prepare 50mL solvent in the volumetric flask, add it to the conical flask, extract, let it stand for precipitation, and take the supernatant after filtration Functional purification column to remove impurities other than other detection items such as fat, pigment and matrix in the sample.

[0034] (1) Optimization of extraction solvent selection

[0035] Methanol, acetonitrile, acetonitrile-water (75:25, V / V) and acetonitrile-water (90:10, V / V) were respectively selected as the extractant to investigate the effect on the extraction effect of AFB1. The results are shown in figure 1 . Depend on figure 1It can be seen that the extraction effect of acetonitrile-water (90:10, V / V) is the best, so this extraction solvent is selected.

[0036] (2) Optimization of extraction time

[0037] A...

Embodiment 3

[0040] Embodiment 3: chromatographic mobile phase ratio optimization

[0041] Use acetonitrile-water solution with a volume of 9:1 as the solvent to prepare a standard solution with a concentration of 5.0ng / mL for the AFB1 standard product, and detect it by UPLC-MS / MS. The mobile phases used are 70:30, 80:20, and 90: 10 and 100:0% acetonitrile-0.1% formic acid water (V / V), observe the total ion flow chromatogram of aflatoxin, the results are shown in Figure 4 . Depend on Figure 4 It can be seen that when using 90:10 acetonitrile-0.1% formic acid water (V / V) as the chromatographic mobile phase, the resulting ultra-high performance liquid chromatogram response value is the highest, the peak type is the most obvious, and there is no tailing and bifurcation. A 90:10 acetonitrile-0.1% formic acid water (V / V) was selected as the chromatographic mobile phase.

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Abstract

The invention belongs to the technical field of analytical testing, and relates to a detection method for aflatoxin B1, in particular to a method for quickly detecting the aflatoxin B1 content in traditional Chinese medicinal materials. The method comprises the following steps that extraction is conducted through an improved QuECHERS method; a solution to be detected is detected through an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer; an aflatoxin B1 standard solution is prepared; a qualitative and quantitative method of the aflatoxin B1 is established. The sample to be detected is quantitatively determined by adopting an external standard method through QuECHERS extraction and ultra-high performance liquid chromatography-triple quadrupole mass spectrometry analysis under the condition of electrospraying ion source ionizing and a multi-reaction monitoring mode. Experimental results show that the method is high in sensitivity, good in stability and suitable for accurate and quick detection for aflatoxin B1 residues in a large quantity of samples and monitor for aflatoxin B1 residues in the traditional Chinese medicinal materials.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, and relates to a detection method for aflatoxin B1, in particular to a method for rapidly detecting the content of aflatoxin B1 in Chinese medicinal materials. Background technique [0002] Aflatoxin (AF) is a kind of toxic secondary metabolites with similar structure produced by fungi such as A. It mainly acts on the liver of humans and animals. There are many kinds of aflatoxins that have been identified. The more common ones are AFB1 and AFB2. Among them, AFB1 is the most toxic. It was listed as a class I carcinogen by the International Agency for Research on Cancer in 1977, and it has great harm. "Pharmacopoeia of the People's Republic of China" (2015 edition) requires that some Chinese medicinal materials such as polygala, jujube, nutmeg, cassia seed, malt, tangerine peel, Shijunzi, Baiziren, and fat sea. Lotus seeds, peach kernels, betel nuts, jujube seeds, coix seeds, etc. m...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 刘艳清汪洪武姚夙严子军韦寿莲罗梓贤
Owner ZHAOQING UNIV
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