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Preparation method of zirconium group hydrophile chromatographic column and application thereof in measuring melamine content in raw milk or dairy product

A hydrophilic chromatographic column and melamine technology, which is applied in the field of chromatographic detection, can solve the problems affecting the sensitivity and accuracy of detection results, cumbersome sample pretreatment operations, and large amount of organic reagents, saving processing time, reducing noise, and standard deviation. small effect

Inactive Publication Date: 2013-02-06
HEBEI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

GB / T22388-2008 HPLC method uses ion-pair chromatography to solve this problem, but the addition of ion-pair reagents not only increases the detection cost, but also causes baseline drift, which affects the sensitivity and accuracy of the detection results
More importantly, the sample pretreatment operation required by this separation mode is very cumbersome, the cycle is long, the detection efficiency is low, the amount of organic reagents is large, and some steps will lead to false positive results.

Method used

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  • Preparation method of zirconium group hydrophile chromatographic column and application thereof in measuring melamine content in raw milk or dairy product
  • Preparation method of zirconium group hydrophile chromatographic column and application thereof in measuring melamine content in raw milk or dairy product
  • Preparation method of zirconium group hydrophile chromatographic column and application thereof in measuring melamine content in raw milk or dairy product

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Experimental program
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Effect test

Embodiment 1

[0039] The preparation of embodiment 1 zirconium-based chromatographic column and the separation of melamine

[0040] Put carefully screened silica gel microspheres with a particle diameter of 3.5 μm (s=0.30) in 6 mol / L hydrochloric acid solution for 0.5 h of sonication for activation pretreatment, suction filtration, washing, and drying. Put the activated and pretreated silica gel microspheres into a 0.1mol / L zirconium solution and magnetically stir for 1.5h for self-assembly to obtain a composite SiO with a layer of zirconia nanoparticles assembled on the surface of the silica spheres. 2 -ZrO 2, suction filtration, washing, and drying; repeat the above operation four times. After burning at 500℃, the core-shell type ZrO can be prepared 2 / SiO 2 microspheres, the ZrO 2 / SiO 2 Zr / Si HILIC was obtained after further flotation of microspheres. Characterized by analysis: Zr / Si HILIC particle size 3.7μm (s=0.31), cylindrical mesopore structure, specific surface area 168.1m ...

Embodiment 2

[0043] Embodiment 2 blank experiment

[0044] Add 8 mL of 1% trichloroacetic acid solution and 2 mL of acetonitrile to a 50 mL plastic centrifuge tube with a stopper, ultrasonically extract for 10 min, shake for 10 min, centrifuge at a speed greater than 4500 r / min for 10 min, take 1 mL of the supernatant and filter it with 0.2 μm Membrane filtration. Perform HPLC determination at room temperature, and quantify with the standard curve method. As a result, no melamine was detected.

[0045] The blank experiment shows that the sample processing process has no interference to the determination of melamine.

Embodiment 3

[0046] The determination of embodiment 3 negative sample and limit of detection

[0047] Accurately weigh 1g (accurate to 0.0001g) negative milk powder sample in a 50mL plastic centrifuge tube with a stopper, add 8mL of 1% trichloroacetic acid solution and 2mL of acetonitrile to the centrifuge tube, ultrasonically extract for 10min, and shake for 10min to obtain a concentration greater than Centrifuge at a speed of 4500r / min for 10min, filter the supernatant through a 0.2μm filter membrane, and perform HPLC determination at room temperature. Quantitatively using the standard curve method, the results did not detect melamine (see figure 2 ).

[0048] Accurately add 0.0100g melamine standard sample to 100g milk powder negative sample, and mix well. Accurately weigh 1g of the sample (accurate to 0.0001g) into a 50mL plastic centrifuge tube with a stopper, use the above method to extract, use the extracted solution as the mother liquor, and measure it by dilution step by step. ...

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Abstract

The invention discloses a zirconium group hydrophile chromatographic column and an application thereof in measuring the melamine content in a raw milk or dairy product. Melamine in a sample is extracted in an ultrasonic, oscillating and centrifuging manner by using a 1% trichloroacetic acid-acetonitrile solution, and HPLC or LC-MS / MS segregation analysis is carried out on sample liquid filtered through a 0.2um filter membrane by using the zirconium group hydrophile chromatographic column. The method for measuring the melamine content in the raw milk or dairy product by using the chromatographic column is simple and convenient, rapid, sensitive and accurate, high in repeatability and low in detection cost. The separating mode is beneficial to the preparation of samples, so that the sample pretreatment is simple in operation, rapid, and high in recovery rate, has no interference on analysis and measurement, the samples can be treated in a batch manner, the time is saved, the measuring cost is reduced, the chromatographic column has long service life, and the indexes are superior to those by using a GB / T22388-2008 method. The method can be widely applied to detecting the melamine in the raw milk or dairy products.

Description

technical field [0001] The invention relates to a preparation method of a zirconium-based hydrophilic interaction chromatographic column and its application in determining the content of melamine in raw milk and dairy products, belonging to the technical field of chromatographic detection. Background technique [0002] Columns are the "heart" of chromatography. An ideal chromatographic column should have good chemical stability and permeability; in addition, the column life of the chromatographic column should be long, so that the repeatability of chromatographic data can be fully guaranteed; the most important thing is that the chromatographic column should be suitable for the components to be measured. The retention effect, the capacity factor k' is preferably in the range of 2-10. [0003] Melamine is a kind of chemical raw material. Because of the high nitrogen content in the molecule, it is called "protein essence". If melamine is contained in dairy products, it may c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60B01J20/283
Inventor 敦惠娟魏雨薛树科宋秀芹谭金标
Owner HEBEI NORMAL UNIV
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