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Method used for screening and identifying saxitoxins in complex matrix

A shellfish toxin and complex matrix technology, applied in the biological field, can solve problems such as lack of qualitative and imperfect screening methods, and achieve the effects of easy operation, lower detection costs, and lower technical level requirements.

Active Publication Date: 2017-07-14
YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the current imperfect screening methods for shellfish toxins in complex matrices and the false positive results caused by lack of quality, the present invention provides a screening and confirmation database and high-resolution confirmation method for shellfish toxins in complex matrices

Method used

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  • Method used for screening and identifying saxitoxins in complex matrix
  • Method used for screening and identifying saxitoxins in complex matrix
  • Method used for screening and identifying saxitoxins in complex matrix

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Embodiment 1

[0035] The technical solutions of the present invention will be further explained below through the embodiments in conjunction with the accompanying drawings, but the scope of protection of the present invention is not conspicuous in any form by the embodiments.

[0036] The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the examples can be obtained from commercial sources unless otherwise specified.

[0037] This example provides a liquid chromatography tandem mass spectrometry database and a high-resolution confirmation method for shellfish toxins in complex matrices, aiming at the current imperfect screening methods for shellfish toxins in complex matrices and the false positive results caused by lack of qualitative properties. Especially the detection method for screening and library confirmation of unknown samples, see figure 1 .

[0038] (1) Preparation of matrix samples

[0...

Embodiment 2

[0058] Embodiment 2 is the qualitative result determination of applying this method in the actual detection process.

[0059] Apply this method to the oyster, scallop, mussel, thick-shelled mussel sample purchased from a certain aquatic product wholesale market in Qingdao, detect by the method of the present invention, the result obtained is as follows:

[0060] Table 5 Contents of 24 shellfish toxins in 4 shellfish samples (μg / kg)

[0061]

[0062]

[0063] in, figure 2 It is the qualitative result decision chart of mussels. image 3 It is the judgment chart of the qualitative results of the thick-shelled mussel.

[0064] Can be compared with the database of shellfish toxin of the present invention, the toxin contained in the sample is shown in Table 5, wherein AZA2 in the thick shell mussel is qualitative (see image 3 ), which was detected by AZA, and the matching degree of the spectral library was 92.5%, which was determined to be detected by AZA2 and then quanti...

Embodiment 3

[0067] Embodiment 3 Method of the present invention compared with traditional quadrupole mass spectrometry detection method results

[0068] 1. The application of this method and the traditional quadrupole mass spectrometry detection method in the detection of false positive samples

[0069] The traditional tandem quadrupole mass spectrometer can only qualitatively analyze the detection results through two pairs of ion pairs, quantitative and qualitative, as shown in the attached figure 2 It can be seen from the test results of the samples in the sample that the deviation of the liquid phase retention time of the target peaks of the two samples is <3%, and the deviation of the ion-to-ion ratio of the two pairs of MRMs is less than 10%. If the ion ratio is qualitative, the sample is an STX positive sample. Through the method adopted in the present invention, a quadrupole-ion trap mass spectrometry is used for detection, and a specific MRM-IDA-EPI mode is applied to obtain a s...

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Abstract

The invention discloses a method used for screening and identifying saxitoxins in complex matrix. The method comprises following steps: 1, preparation of a matrix sample; 2, matrix sample purification, and toxin separation; 3, establishment of a mass spectrometry database; 4, sample information acquisition and result determination; 5, high resolution mass spectrum measuring of suspected positive samples and metabolic products of the suspected positive samples; and 6, qualitative measurement used for determining accurate molecule mass. According to the method, the mass spectrometry databases of 24 kinds of saxitoxins are established, the method can be used for high precision qualitative analysis in sample screening processing, realizing blind measuring of toxic-free standard samples and accurate qualitative determination, solving problems in the prior art that standard substances are expensive, arrival period is long, and the standard substances are controlled by entry and exit administration, and reducing detection cost in daily monitoring; requirement on the technical level of operation staff in saxitoxin detection is reduced; and operation is convenient.

Description

technical field [0001] The invention relates to a screening and confirmation database of shellfish toxins in complex matrix and a high-resolution confirmation method, belonging to the field of biotechnology. Background technique [0002] my country has abundant marine ecological resources and aquaculture resources. With the intensification of coastal environmental pollution, harmful algal blooms and associated shellfish toxins have become one of the major food safety issues. Due to the pollution of shellfish toxins, since the 1990s, developed countries led by the European Union have banned the import of shellfish to my country, which has caused huge economic losses to my country's shellfish industry. In recent years, there have been many incidents of group poisoning and even death due to the contamination of bivalve molluscs with shellfish toxins. Mussel paralytic toxin poisoning incident in Qinhuangdao, etc. What's more, the two abnormal phenomena of normality and univers...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 吴海燕谭志军郭萌萌郑关超彭吉星翟毓秀
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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