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Pretreatment device and method for sulfonamide antibiotic detection of aquatic products and application

A technology for sulfonamides and antibiotics, which is applied in the field of pretreatment devices for the detection of sulfonamides antibiotics in aquatic products, can solve the problems of time-consuming and laborious, long time-consuming nitrogen blowing and concentration, cumbersome steps, etc., and achieve sensitive and reliable analysis basis and analysis method, purification and removal The effect of good miscellaneous effect and accurate measurement result

Pending Publication Date: 2019-01-25
太湖流域水文水资源监测中心
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The disadvantage of using this method for purification is that the main function of n-hexane is to degrease the sample, but the sample also contains some substances such as polar phospholipids and / or glycoproteins, which cannot be degreased under the action of n-hexane. However, the polar phospholipids and / or glycoproteins remaining in the sample will also produce matrix effects and affect the accuracy of the test results.
Moreover, n-hexane is used as a degreasing agent, and its degreasing and purification effect is not ideal. After the degreasing operation of n-hexane, the extract still contains a small part of non-polar lipids, and these unremoved lipids will also cause matrix effect , affecting the accuracy of the test results
[0006] At the same time, these residual proteins and lipids in the sample will not only affect the accuracy of the test results, but also increase the difficulty of the detection of antibiotics in aquatic products, and because the samples contain proteins and lipids, it is easy to cause chromatographic Unfavorable results such as increased column pressure, blockage of the ion source nozzle of the mass spectrometer, and contamination of the cone and pre-quadrupole greatly shorten the service life of the detection equipment
[0007] In order to reduce the residue of proteins and lipids and improve the purification effect, the existing purification operation is not only cumbersome, but also requires the use of a large amount of acetonitrile and other toxic reagents, and the consumption of solid-phase extraction consumables is large during the purification process. Time-consuming and difficult to manipulate manually
Not only is it time-consuming and labor-intensive, but it is also limited by excessive drying during the pretreatment process, resulting in the loss of target compounds, so the purification effect is poor, the repeatability of samples between batches is poor, and the accuracy of quantitative results is unstable.

Method used

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  • Pretreatment device and method for sulfonamide antibiotic detection of aquatic products and application
  • Pretreatment device and method for sulfonamide antibiotic detection of aquatic products and application
  • Pretreatment device and method for sulfonamide antibiotic detection of aquatic products and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] First, assemble the pretreatment device for the detection of sulfonamide antibiotics in aquatic products in the following manner, including four six-way valves, respectively No. 1 valve 11, No. 2 valve 22, No. 3 valve 33, and No. 4 valve 44, wherein each Each six-way valve has six ports, the No. 5 port 11 (5) of the No. 1 valve 11 is connected with the No. 1 port 22 (1) of the No. 2 valve 22 through pipelines, and the No. 4 port of the No. 1 valve 11 11(4) is connected with No. 2 port 44(2) of No. 4 valve 44 through a pipeline, and between No. 3 port 33(3) of No. 3 valve 33 and No. 3 port 44(3) of No. 4 valve 44 It also includes a mixer 55, the mixer 55 has two inlets and an outlet, the first inlet 55 (1) of the mixer 55 and the third interface 22 (3) of the second valve 22 are connected through pipelines, the No. 2 inlet 55-2 of the mixer is connected with the No. 6 interface 44(6) of the No. 4 valve 44 through a pipeline, and the outlet 55(3) of the mixer 55 is connec...

Embodiment 2

[0090] The samples treated with Example 1 and Comparative Example 1 were respectively tested for sulfa antibiotics.

[0091] In this example, we detected 18 common sulfonamide antibiotics, see Table 1 for details:

[0092] Table 1:

[0093]

[0094]

[0095]

[0096] Standard solution preparation

[0097] Prepare 1.0ng / L, 5.0ng / L, 10.0ng / L, 20.0ng / L, 50.0ng / L standard solutions with 0.1moL / L hydrochloric acid aqueous solution, inject 1mL of each concentration, and take the peak area as horizontal Coordinates, the concentration is the ordinate to draw a standard curve, and the limit of detection (LOD) is calculated with 3 times the signal-to-noise ratio (S / N) (see Table 2). The linear correlation coefficient is not less than 0.998.

[0098] Linear curves such as Figure 22 As shown, among them,

[0099]

[0100]

[0101] See the experimental results figure 2 and image 3 . according to figure 2 with image 3 We can clearly see that the liquid chromato...

Embodiment 3

[0103] The mensuration of the sample recovery rate of the method disclosed by the invention

[0104] Prepare a water sample, measure 7 parts, each 10mL. Label, 0-6. Sample No. 0 is set as blank, each sample of No. 1-3 is added with 5.0ng / L standard; No.3-6, each sample is added with 50.0ng / L standard. Sample recovery experiments with low and high concentrations were carried out, and the sample recovery rate was calculated by subtracting the concentration of the analyte in the blank sample from the concentration of the analyte in the standard added sample and the concentration of the analyte added. The results are shown in Table 2.

[0105] Measurement of Sample Precision of the Method Disclosed in the Invention

[0106] Prepare a water sample, measure 8 parts, each 10mL. Label 0-7, set sample 0 as blank, and add 10.0ng / L standard to samples 1-7; calculate the relative standard deviation of the sample by subtracting the concentration of the analyte in the blank sample from th...

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Abstract

The invention relates to the field of aquatic product quality monitoring, in particular to the field of monitoring of antibiotics in the aquatic products and more particularly relates to a pretreatment device and method for sulfonamide antibiotic detection of aquatic products and application. By establishment of an online solid-phase extraction and elution pretreatment device for online enrichmentand purification of sulfonamide antibiotics and an online enrichment and purification pretreatment method based on the device, high automation in pretreatment and low loss of the sulfonamide antibiotics in a pretreatment process can be realized. By the method, automatic online purification of complex substrate samples can be realized, high analysis efficiency, low acetonitrile solvent consumption, great purification and decontamination effects, high accuracy and reproducibility of determination results and the like are realized, and the simple, convenience, sensitive and reliable analysis foundation and analysis method are provided for determination of sulfonamides in the aquatic products.

Description

technical field [0001] The invention relates to the field of quality monitoring of aquatic products, in particular to the field of monitoring antibiotics in aquatic products, and more specifically relates to a pretreatment device, method and application for detection of sulfonamide antibiotics in aquatic products. Background technique [0002] Aquatic products are the general term for aquatic animal and plant products and their processed products produced by marine and freshwater fisheries. In the process of aquaculture, in order to prevent and control aquaculture diseases, it is necessary to use antibiotics and other prevention and control drugs. Sulfonamides are commonly used antibiotic fishery drugs for prevention and control. At present, the abuse of antibiotics occurs frequently, and sulfonamide antibiotics can be accumulated and stored in aquatic products, posing a threat to aquatic ecosystems. [0003] In order to prevent the abuse of antibiotics, especially sulfona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/24G01N30/14G01N30/34G01N30/32G01N30/08G01N30/02G01N30/72
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N30/24G01N30/32G01N30/34G01N30/72G01N2030/324G01N2030/067G01N2030/062Y02A40/81
Inventor 李涛石亚东徐枫徐兆安虞霖
Owner 太湖流域水文水资源监测中心
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