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Detection reagent combination and detection method for aquatic product additives

A detection reagent and detection method technology, which is applied in the detection reagent combination and detection field of aquatic additives, can solve the problems of large sample matrix interference and high detection limit of the method, achieve low false negative and false positive rate, wide detection range, and ensure correctness sexual effect

Active Publication Date: 2018-11-20
INST OF CHINESE MATERIA MEDICA CHINA ACAD OF CHINESE MEDICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

High performance liquid chromatography has the limitations of high detection limit and large sample matrix interference

Method used

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  • Detection reagent combination and detection method for aquatic product additives
  • Detection reagent combination and detection method for aquatic product additives
  • Detection reagent combination and detection method for aquatic product additives

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Experimental instruments and reagents

[0047] 1.1 Experimental Instruments

[0048] AcQuity TM UPLC ultra-high pressure liquid chromatograph was purchased from Waters in the United States, API5500Qtrap mass spectrometer was purchased from AB in the United States, vortex mixer, TTL-DC II nitrogen blowing instrument, IKA high-speed tissue homogenizer, ultrapure water instrument (Simplicity, Merck Millipore) company), ultrasonic extractor (KQ-250B, Kunshan Ultrasonic Instrument Co., Ltd.), IKAT18Basic high-speed dispersing machine (Germany).

[0049] 1.2 Reagents

[0050] Methanol (chromatographically pure), acetonitrile (chromatographically pure) formic acid has a purity of 99%, nitrofuran metabolites (purity ≥ 99%): furaltadone metabolite (AMOZ), nitrofurazone metabolite (SEM), nitrofurantoin metabolite ( AHD), furazolidone metabolite (AOZ) were purchased from Dr.Ehrenstorfer GmbH, Germany.

[0051] 2. Method

[0052] 2.1 Sample pretreatment

[0053] Accurately...

Embodiment 2

[0078] Actual sample analysis

[0079] The blank samples and actual test samples used in the experiment were purchased from the market in Shandong Province. After processing, they were stored in a refrigerator at 4°C for later use.

[0080] Use this method to detect 10 freshwater fish samples purchased (the total ion chromatogram of additives in aquatic products is shown in figure 1 Shown), found 1 case of positive samples, detected, nitrofurazone metabolite content was 0.41ng / mL, see figure 2 .

[0081] The invention adopts high-performance liquid chromatography tandem mass spectrometry technology to establish an analysis method for nitrofuran metabolites in aquatic products in aquatic products. The method is simple, fast, sensitive, specific, and reproducible. It can simultaneously determine four nitrofuran metabolites in aquatic products, realizes its high-throughput analysis, and can meet the monitoring requirements of additives in aquatic products.

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Abstract

The invention discloses a detection reagent combination and a detection method for aquatic product additives. An aqueous solution of acetonitrile containing nitrofuran metabolites is used as a reference substance; a methanol mixture containing a methanol solution of 2-nitrobenzaldehyde and an aqueous solution of hydrochloric acid is used as a derivatizing agent; and a liquid chromatography-tandemmass spectrometry method is used for detection. The detection reagent combination provided by the invention can simultaneously analyze additives in aquatic products, and has the widest detection range; a scheme of simultaneous derivatization of protein precipitates is adopted in sample treatment to directly derivatize, purify and enrich the nitrofuran metabolites in biological samples and shortenthe derivatization time of a traditional method from 16 h to 10-20 min; and the detection method using the reagent combination is simple, accurate, rapid, stable, free from enzymatic conversion and other complicated steps, free from interference of endogenous substances on detection results, low in false negative rate and false positive rate, low in reagent cost, and suitable for rapid analysis ofa large number of samples.

Description

technical field [0001] The invention relates to the technical field of additive detection, in particular to a detection reagent combination and a detection method for aquatic additives. Background technique [0002] The problem of nitrofuran drug residues in aquatic products is one of the food safety hotspots that are generally concerned by countries all over the world. Establishing effective drug residue analysis methods is the premise and basis for monitoring and controlling drug residues in aquatic products. Due to the complexity of the substrate of aquatic products and the particularity of aquaculture drugs, there are some difficulties and problems in the detection of drug residues in aquatic products. On the one hand, relevant laws and regulations have set limit requirements for some newly emerging or newly used drugs in aquaculture, but there is a lack of suitable detection methods. On the other hand, some existing multi-residue detection methods have long detection ti...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李鹰飞吴思玚
Owner INST OF CHINESE MATERIA MEDICA CHINA ACAD OF CHINESE MEDICAL SCI
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