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Method for detecting tripolycyanamide in aquatic product via pressurized capillary electrochromatography

A capillary electrochromatography and melamine technology, which is applied in the field of food safety and veterinary drug residues, can solve the problems of long analysis time, low sensitivity of liquid chromatography, difficult to configure instruments, etc., and achieves high efficiency of the analysis method, less consumption of organic reagents, and high sensitivity. Effect

Inactive Publication Date: 2012-08-29
NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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Problems solved by technology

The sensitivity of liquid chromatography is low, and the analysis time is long. Although the detection sensitivity and resolution of gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry are high, it is difficult for general laboratories to configure such instruments

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  • Method for detecting tripolycyanamide in aquatic product via pressurized capillary electrochromatography
  • Method for detecting tripolycyanamide in aquatic product via pressurized capillary electrochromatography
  • Method for detecting tripolycyanamide in aquatic product via pressurized capillary electrochromatography

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Embodiment Construction

[0024] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.

[0025] In this embodiment, taking saury as an example, capillary electrochromatography is used to detect residual melamine in saury, and the specific steps are:

[0026] 1. Sample preparation: Cut the saury muscle tissue sample with scissors, homogenize it, and freeze it;

[0027] 2. Sample pretreatment:

[0028] (1) Extraction: thaw the sample, accurately weigh 2±0.01g (accurate to 0.01g) homogeneous sample and place it in a 50mL centrifuge tube, add 10mL of 1% trichloroacetic acid and 5mL of acetonitrile, and use a vortex mixer to fully Mix well for 1-2min, centrifuge at 5000r / min for 10min, collect the supernatant, then add 15mL of a mixture of 1% trichloroacetic acid and acetonitrile with a volume ratio of 2:1 to the original centrifuge tube to repeat the extraction once, and combine the supernatant twice .

[0029] (2) Purification: Us...

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Abstract

The invention relates to a method for detecting tripolycyanamide in an aquatic product via pressurized capillary electrochromatography, which comprises the steps of: 1) sample preparation; 2) sample pretreatment: centrifugal extraction of a sample by mixed solution of trichloroacetic acid with the mass concentration of 0.8-1.2 percent and acetonitrile at the volume ratio of (1.5-2.5):1, purification by an MCX (methoxycinnamate) solid-phase extraction column, and filtration by a filter film of 0.20-0.24mum for determination via the pressurized capillary electrochromatography; 3) preparation of standard tripolycyanamide solution; 4) analysis via the pressurized capillary electrochromatography; and 5) detection and analysis of the sample, quantitative analysis according to the retention time, and then quantitative analysis in an external marking method according to the peak area. The analytical method is efficient, accurate and highly sensitive, and the demands of drug detection of the tripolycyanamide in the daily aquatic product can be satisfied.

Description

technical field [0001] The invention relates to the field of food safety-veterinary drug residues, specifically an analysis method for detecting melamine in aquatic products by using a capillary electrochromatograph. Background technique [0002] Melamine, referred to as triamine for short, is a triazine nitrogen-containing heterocyclic organic compound, and its main purpose is to produce melamine formaldehyde resin. Because the mass fraction of nitrogen is about 66%, some unscrupulous manufacturers add a large amount of crude protein in the feed to increase the crude protein content in the product. After aquatic organisms eat feed containing melamine, it may be enriched in the body, which seriously damages the health and safety of consumers. Benefit. The "Sanlu milk powder incident" in September 2008 aroused people's attention to melamine. However, the currently released methods only have the detection method of melamine in raw milk and dairy products and the detection me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 曹国洲朱晓艳肖道清刘在美杨文潮陈少鸿郑琳陈建国董洁莹
Owner NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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