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Method for simultaneously measuring malachite green and crystal violet residual quantity in aquaculture water

A malachite green and aquaculture water technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inaccurate qualitative and low recovery rate, and achieve the effects of accurate qualitative and quantitative, efficient process and high sensitivity

Inactive Publication Date: 2017-12-12
大连市水产技术推广总站
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] High-performance liquid chromatography is qualitative by retention time and quantitative by external standard method, which has the disadvantage of inaccurate qualitative and low recovery rate

Method used

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  • Method for simultaneously measuring malachite green and crystal violet residual quantity in aquaculture water
  • Method for simultaneously measuring malachite green and crystal violet residual quantity in aquaculture water
  • Method for simultaneously measuring malachite green and crystal violet residual quantity in aquaculture water

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Embodiment 1

[0060] Example 1 Determination of residual malachite green and crystal violet in nursery pond water.

[0061] 1. Instruments and equipment used in this embodiment: LC-MS / MS liquid chromatography tandem mass spectrometer

[0062] (1) Liquid chromatography part (I-class of Waters Company), using Waters BEH C18 reverse phase chromatographic column, (2.1mm╳100mm, 1.7μm)

[0063] (2) TQ-S mass spectrometer (Waters company), equipped with ESI ion source, triple quadrupole, collision cell, vacuum system, gas path control system;

[0064] (3) Electronic balance: Sensitivity 0.01mg (Sartorius, Germany)

[0065] (4) Solvent filter: equipped with 0.45μm water filter membrane (Tianjin Jinteng Company)

[0066] (5) Rotary evaporator (BUCHI company)

[0067] (6) Vortex mixer (Germany IKA company)

[0068] (7) Solid phase extraction instrument (Waters company)

[0069] (8) Ultrapure water meter (Sartorius, Germany)

[0070] (9) Microporous filter membrane: 0.22 μm, nylon 66 pinhole fil...

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Abstract

The invention provides a method for simultaneously measuring malachite green and crystal violet residual quantity in aquaculture water. The method comprises the following steps: using an isotope corresponding to a target compound as an interior label, filtering a water sample, concentrating by the liquid-liquid extraction, purifying by a neutral alumina column, executing the constant volume by using acetonitrile-ammoniumacetate solution after the concentration, and detecting by using a liquid chromatograph / mass spectrometer after the vortex vibration filtration. The method is capable of simultaneously measuring the malachite green and crystal violet in the aquaculture water by using the liquid chromatograph / mass spectrometer firstly, so the sensitivity is high, the qualitative analysis is reliable, and the quantification is accurate. The method is capable of detecting the malachite green and crystal violet in the water by using a liquid chromatography-mass spectrometry interior label method which is used for effectively correcting the error and loss in the pre-treating process and of which the recovery rate is higher and stable, so the measuring result is accurate and reliable, the sensitivity is high, the repeatability is good, and the quantification is accurate. The technical support is provided for relevant departments for monitoring the illegal use of the malachite green and crystal violet in the aquaculture. The method has the good application prospect.

Description

technical field [0001] The invention belongs to the technical field of environmental quality and safety detection, and relates to a method for simultaneously detecting residual amounts of malachite green and crystal violet in aquaculture water by using high-performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Malachite green, also known as alkaline green, strict block green, malachite green, is a green crystal with metallic luster, commonly used as a dye in industry; crystal violet is used as a stain in cytology, histology and bacteriology. The application is extremely wide. In aquaculture, fishermen often use malachite green and crystal violet to disinfect water bodies, kill parasites, and prevent fish saprolegniasis, gill mold disease, and melon worm disease. They are also used as disinfectants during the transportation of fish and when they are temporarily raised and sold in fish tanks in markets and restaurants to prolong the surviva...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 丁勇张秀妍王骏
Owner 大连市水产技术推广总站
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