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Method for quick detection of content of citrinin in traditional Chinese medicinal materials

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

Inactive Publication Date: 2016-09-21
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 quick detection of content of citrinin in traditional Chinese medicinal materials
  • Method for quick detection of content of citrinin in traditional Chinese medicinal materials
  • Method for quick detection of content of citrinin in traditional Chinese medicinal materials

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: the method for rapid determination of citrinin content in Chinese herbal medicine of the present invention

[0023] The rapid determination method of the present invention is applicable to the rapid detection of citrinin content in Chinese herbal medicine sample, and this method comprises the following steps:

[0024] (1) QuEChERS extraction: Take 5.00 g of sample powder with a particle size of 0.02 mm after crushing and grinding, add it to a 100 mL conical flask, prepare 50 mL of acetonitrile-water (volume ratio: 75:25) solution in the volumetric flask, and add it to the conical flask In a shaped bottle, shake at 350r / min for 25min, let it stand for precipitation, and after filtration, take the supernatant to pass through a purification column, concentrate and pass through a 0.22μm filter membrane before testing.

[0025] (2) Preparation of citrinin standard solution: Accurately weigh 5.0mg citrinin (CIT) standard product in a 100.00mL volumetric flask, d...

Embodiment 2

[0030] Embodiment 2: the improvement of QuEChERS extraction method

[0031] Take the sample and grind it to get 5.00g of powder with a particle size of 0.02mm, add it to a 50mL conical flask, prepare 25mL solvent in the volumetric flask, add it to the conical flask, extract, let it stand for precipitation, filter and take the supernatant for purification The column removes impurities other than other detection items such as fat, pigment and matrix in the sample.

[0032] (1) Optimization of extraction solvent selection

[0033] Methanol, acetonitrile, acetonitrile-water (75:25, V / V) and acetonitrile-water (80:20, V / V) were respectively selected as extractants to investigate the effect on the extraction effect of CIT. The results are shown in figure 1 . Depend on figure 1 It can be seen that the extraction effect of acetonitrile-water (75:25, V / V) is the best, so this extraction solvent is selected.

[0034] (2) Optimization of extraction time

[0035] Acetonitrile-water (...

Embodiment 3

[0038] Embodiment 3: chromatographic mobile phase ratio optimization

[0039] Use acetonitrile-water solution with a volume of 6:4 as a solvent to prepare a standard solution with a concentration of 5.0ng / mL for the CIT standard substance, and detect it with UPLC-MS / MS. :4, 7:3, 8:2 and 9:1 acetonitrile-0.1% formic acid in water and 6:4, 7:3, 8:2 and 9:1 acetonitrile-5mM ammonium acetate buffer saline pair 5.0ng / mL citrinin standard solution to detect the peak-out situation of citrinin, observe the total ion current chromatogram of CIT, the results are shown in Figure 4 . Depend on Figure 4 It can be seen that when using 8:2 acetonitrile-5mM ammonium acetate buffer salt as the mobile phase of ultra-high performance liquid chromatography, the resulting ultra-high performance liquid chromatography has the highest response value, the best peak shape, and the most stable baseline. When no other mobile phase is used The occurrence of trailing fork and so on. Therefore, 8:2 ac...

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Abstract

The invention belongs to the technical field of analytical testing and relates to a citrinin detection method, in particular to a method for quick detection of the content of citrinin in traditional Chinese medicinal materials. The method comprises the steps of extraction with an improved QuEChERS method, detection of liquid to be detected by means of an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer, preparation of citrinin standard solution, and establishment of a citrinin quality and quantity determination method. The sample to be detected is subjected to QuEChERS extraction and ultra-high performance liquid chromatography-triple quadrupole mass spectrometer (UPLC-MS / MS) analysis, and then quantitative determination is conducted with an external standard method under the condition of electrospray ionization and multi-reaction monitoring mode. Experiment results show that the method is high in sensitivity and stability, and is suitable for accurate and quick detection of citrinin residues in a large number of samples and detection of citrinin residues in 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 of citrinin, in particular to a method for rapidly detecting the content of citrinin in Chinese medicinal materials. Background technique [0002] Citrinin (Citrinin, CIT), also known as citrinin, is a mycotoxin produced by certain strains of Penicillium and Aspergillus. , The metabolic process of Monascus exists in grains, fruits, meat and related products. With the development of the times, the pollution of Bummycin in food is becoming more and more serious. After human beings eat some contaminated food for a long time, Blightymycin will accumulate in the body in large quantities, causing renal organ lesions, and even leading to cysts and tumors. People's health is seriously threatened. [0003] At present, the main detection methods of citrinin include liquid chromatography, enzyme-linked immunosorbent assay, thin-layer chromatography and liquid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 刘艳清汪洪武姚夙严子军韦寿莲黄晓真
Owner ZHAOQING UNIV
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