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

CN102628844AInactive Publication Date: 2012-08-08HUNAN INST FOR FOOD & DRUG CONTROL
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2012-08-08
Estimated Expiration
Not applicable · inactive patent

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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.
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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...

Examples

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...