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Liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxins in shellfish

A liquid chromatography and shellfish toxin technology, which is applied in the field of liquid chromatography-tandem mass spectrometry detection of paralytic shellfish toxins, can solve the problems of cumbersome degreasing steps, high consumption, limited types of PSTs components, etc., and broaden the detection types , fewer interference peaks, and shortened preprocessing time

Pending Publication Date: 2021-02-19
SHENZHEN CENT FOR DISEASE CONTROL & PREVENTION +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the degreasing step of this liquid chromatography-tandem mass spectrometry method is cumbersome, requires a large amount of organic solvents such as ethyl acetate, and the types of PSTs components that can be quantitatively detected are relatively limited.

Method used

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  • Liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxins in shellfish
  • Liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxins in shellfish
  • Liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxins in shellfish

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxin in shellfish

[0048] A liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxin in shellfish, comprising the steps of:

[0049] 1.1 Sample extraction: Take 5g of shellfish sample in a 50mL centrifuge tube, add 8mL of 0.5% by volume formic acid solution, vortex and mix for 5min, ultrasonically extract for 10min, centrifuge at 9500r / min for 10min, take the supernatant, Use 0.5% by volume formic acid solution to dilute to 10mL to obtain sample extract;

[0050] 1.2 Purification of the sample: Take 2mL of the sample extract in a 15mL centrifuge tube, add 5mL of dichloromethane, vortex and mix for 3min, centrifuge at 9500r / min for 5min, take 1mL of the supernatant and add 3mL of acetonitrile and 3mL of 0.5% In a C18 solid-phase extraction column activated by formic acid solution, elute with 1.5mL of 0.5% formic acid solution, collect ...

Embodiment 2

[0056] Example 2 Linearity and detection limit of liquid chromatography-tandem mass spectrometry detection method

[0057] In order to eliminate the matrix effect, 13 kinds of PSTs were prepared into matrix standard working solutions with different concentration gradients by using blank matrix in this experiment. The chromatograms of the standard working solutions of 13 kinds of PSTs components are shown in Figure 1-Figure 13 shown. Take the concentration of the working solution as the abscissa, and the quantitative ion peak area as the ordinate to draw the matrix standard curve of 13 kinds of PSTs components. The results are shown in Table 4. The linear correlation coefficient (r 2 ) were higher than 0.99, indicating a good linear relationship. When the signal-to-noise ratio of the low-concentration target is greater than or equal to 3 (S / N≥3), the lowest concentration that meets this condition is taken as the detection limit (LOD) of the corresponding target; when the sign...

Embodiment 3

[0060] Example 3 Recovery and precision of liquid chromatography-tandem mass spectrometry detection method

[0061] Three different concentrations of PSTs mixed standard solutions were added to the blank shellfish samples, and three parallels were set for each addition level. The results are shown in Table 5. The measured recoveries of PSTs ranged from 53.65% to 122.95%. Except for the low levels of C1, dcGTX2 and GTX3, the method recoveries of other toxins were all in the range of 60% to 120%. The precision of the method measured by three parallel experiments was 0.98%-16.74%.

[0062] Table 5 Part of the PSTs component spike recovery and detection precision

[0063]

[0064] In summary, the liquid chromatography-tandem mass spectrometry detection method of paralytic shellfish toxin in shellfish provided by the present invention has realized the detection of 13 kinds of PSTs components such as STX, is easy to operate, reduces the consumption of organic solvents, and the d...

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Abstract

The invention provides a liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxins in shellfish. The method comprises the following steps: 1.1, performing sample extraction: adding a formic acid solution into a shellfish sample, carrying out ultrasonic extraction and centrifuging, taking the supernatant, and fixing the volume to obtain a sample extracting solution; 1.2, performing sample purification: adding dichloromethane into the sample extracting solution, uniformly performing mixing, performing centrifuging, taking supernatant, adding the supernatant into an activated C18 solid-phase extraction column, performing eluting, collecting effluent and eluent, performing combining, fixing the volume, performing standing, performing centrifuging, and taking a supernatant filter membrane to obtain a sample detection solution; and 1.3, performing sample detection: taking the sample detection solution, carrying out liquid chromatography-tandem mass spectrometry detection, and performing quantifying by an external standard method. The method belongs to the technical field of food safety detection, simplifies the operation, reduces the consumption of anorganic solvent, has a good sample purification effect, does not need an ultrafiltration step, realizes effective separation and detection of partial structural analogues in PSTs, and widens the detection variety of the PSTs.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, in particular to a liquid chromatography-tandem mass spectrometry detection method for paralytic shellfish toxin in shellfish. Background technique [0002] Shellfish toxins generally refer to marine biotoxins that are enriched and transmitted by shellfish. According to the existing recorded symptoms and exposure medium, the poisoning caused by marine biotoxins can be divided into paralytic shellfish poisoning (PSP), neurotoxic shellfish poisoning (Neurotoxic Shellfish Poisoning, NSP), amnesia Shellfish poisoning (Amnestic Shellfish Poisoning, ASP), diarrhea shellfish poisoning (Diarrhetic Shellfish Poisoning, DSP) and Xijia fish poisoning (Ciguatera Fish Poisoning, CFP). [0003] Paralytic shellfish toxins (PSTs), which can accumulate in aquatic organisms such as filter-feeding bivalve molluscs and crustaceans, are the most widely distributed and most harmful type of marine biotox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14G01N30/86
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N30/8675G01N2030/047G01N2030/062G01N2030/146
Inventor 刘建军黄柏强黄科张建莹陈效周彦
Owner SHENZHEN CENT FOR DISEASE CONTROL & PREVENTION
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