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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  • Abstract
  • Description
  • Claims
  • Application Information

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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
E

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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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Example Embodiment

[0023] Example 1: The method of the present invention for rapidly determining the content of aflatoxin B1 in Chinese medicinal materials

[0024] The rapid determination method of the present invention is suitable for rapid determination of the content of aflatoxin B1 in traditional Chinese medicinal materials, and the method includes the following steps:

[0025] (1) QuEChERS extraction: Take 5.00g Chinese medicinal material sample, pulverize and grind to obtain sample powder with a particle size of 0.02mm, add it to a 100mL conical flask; prepare 50mL acetonitrile-water (volume ratio 90:10) solution in a volumetric flask , Added to the conical flask, oscillated at 350r / min for 25min, allowed to stand for precipitation, filtered, took the supernatant through the purification column, concentrated it through a 0.22μm filter membrane for testing;

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

[0027] ...

Example Embodiment

[0032] Example 2: Improvement of QuEChERS extraction method

[0033] Take the sample and grind it to obtain 5.00g of powder with a particle size of 0.02mm, add it to a 100mL conical flask, prepare 50mL solvent from the volumetric flask and add it to the conical flask, extract, let stand for precipitation, filter and take too much supernatant The functional purification column removes the fat, pigment, matrix and other impurities outside the test items 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 selected as extractants to investigate the effect on the extraction effect of AFB1. The results are shown in figure 1 . by figure 1 It can be seen that acetonitrile-water (90:10, V / V) has the best extraction effect, so this extraction solvent is selected.

[0036] (2) Optimization of extraction time

[0037] Acetonitrile-water (90:10, V / V) was used as the extrac...

Example Embodiment

[0040] Example 3: Optimization of chromatographic mobile phase ratio

[0041] Use acetonitrile-water solution with a volume of 9:1 as the solvent to prepare a standard solution with a concentration of 5.0 ng / mL for the AFB1 standard. UPLC-MS / MS detection, respectively, use mobile phases of 70:30, 80:20, 90: 10 and 100:0% acetonitrile-0.1% formic acid water (V / V), observe the total ion current chromatogram of aflatoxin, see the result Figure 4 . by Figure 4 It can be seen that when 90:10 acetonitrile-0.1% formic acid water (V / V) is used as the chromatographic mobile phase, the ultra-high performance liquid chromatogram obtained has the highest response value, the most obvious peak shape, and no tailing and bifurcation. Choose 90:10 acetonitrile-0.1% formic acid water (V / V) 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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