Content determining method for trichlorfon in dried fish

A determination method and trichlorfon technology are applied in the field of detection of trichlorfon residues in dried fish, which can solve the problems of high operation cost, many impurities and interference in determination of liquid chromatography-mass spectrometer, and reduce false positives. Probability of results, high detection sensitivity, effect of increased purification steps

Inactive Publication Date: 2012-08-08
HUNAN INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

There are many impurities in the processed sample solution, and there are many miscellaneous peaks in the gas chromatogram, which interfere with the measurement
Moreover, there are still a large amount of oil components in the sample solution, which are not easy to volatilize and accumulate in the injection port, which will contaminate the liner and other sampling systems, and easily cause cross-contamination to the measurement
2. The determination method of SNT 1920-2007 is only for the determination of trichlorfon in fresh meat, casings and honey. After extracting trichlorfon with dichloromethane, concentrate to dryness, dissolve the residue with acetonitrile, and add a small amount of cyclohexane to remove it. fat
There are also a lot of impurity interference, and the operation cost of liquid mass spectrometry is high, and a large amount of organic solvents required for the mobile phase are likely to pollute the environment

Method used

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  • Content determining method for trichlorfon in dried fish
  • Content determining method for trichlorfon in dried fish
  • Content determining method for trichlorfon in dried fish

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1 Reagents and materials

[0038] 1.1 Liquid reagents: acetonitrile (chromatographically pure), chloroform (chromatographically pure), ethyl acetate (chromatographically pure), n-hexane (pesticide residue grade)

[0039] 1.2 Solid reagent: anhydrous sodium sulfate (analytical pure), zinc acetate (analytical pure)

[0040] 1.3 Purified water

[0041] 1.4 Experimental equipment: sampling bottle, centrifuge tube (50ml), precision adjustable pipette gun (100-1000μl, 10-100μl), volumetric flask, concentration bottle (250ml), separatory funnel (250ml)

[0042] 1.5 Standard product: the purity of trichlorfon is above 98.0%

[0043] 2 Instruments and analysis conditions:

[0044] 2.1 Agilent 7890N / 5975C Gas Chromatograph / Mass Spectrometer

[0045] 2.2 Rotary evaporator

[0046] 2.3 Homogenizer

[0047] 2.4 Vortex mixer

[0048] 2.5 Centrifuge (5000r / min)

[0049] 2.6 Balance: Accuracy 10mg / 0.01mg, used for weighing the test product and standard product

[0050] 3 Sampl...

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Abstract

The invention belongs to the technical field of content determination of trichlorfon, and provides a content determining method for trichlorfon in dried fish. The method comprises the following specific steps of: (1) preparing a standard curve; (2) preparing a sample solution, to be specific, (1) pretreating; (2) extracting; (3) concentrating; and (4) purifying; and (3) detecting the sample with a gas chromatography-mass spectrometry method. Compared with the prior art, the method has the advantages that: during preparation of the sample solution, a purifying step in a pretreatment process is mainly increased, so that the interference of greasy substances in the sample on determination is greatly lowered, and the probability of a false positive result is lowered; and trichlorfon is detected by using the gas chromatography-mass spectrometry method, so that determination is accurate, and the detection sensitivity is high.

Description

technical field [0001] The invention belongs to the field of content determination of trichlorfon, and is suitable for detecting the residual amount of trichlorfon in dried fish. Background technique [0002] Trichlorfon is an insecticide with high efficiency, low toxicity and low residue. It has a good killing effect on trematodes, nematodes, acanthocephalans parasitic inside and outside fish, and harmful fish fry, cladocerans, radial horns, mussel larvae and water centipedes. However, because trichlorfon can form dichlorvos with greater residual toxicity under weakly alkaline conditions, when the pH value is 8-10, it only takes half an hour for trichlorfon to transform into dichlorvos. Therefore, not only the toxic effects of fish and shrimp must be taken into consideration, but also the safety of humans and animals cannot be ignored. [0003] In recent years, my country has repeatedly found that illegal traders use trichlorfon to process salted fish, which has brought g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 吴公平殷帅刘雁鸣林海廖彬
Owner HUNAN INST FOR FOOD & DRUG CONTROL
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