Thin-layer chromatographic developer for detecting residual amount of tripolycyanamide and application of thin-layer chromatographic developer

A technology of thin-layer chromatography and melamine, which is applied in the field of thin-layer chromatography color reagents, can solve the problems of insufficient sensitivity and failure to meet the detection requirements of melamine, and achieve the effects of high detection sensitivity, clear spots and simple operation

Inactive Publication Date: 2011-09-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Melanie Broszat etc. used Wuster's blue and starch iodine reagent as chromogenic reagents to check melamine in milk (A new method for quantification of melamine in milk by absorption diode-array thin-layer chromatography. Journal of Planar Chromatography, 2008, 21(6) : 469), the detection limit was 30mg·L -1 , the sensitivity is not high enough to meet the detection requirements of trace amounts of melamine in food

Method used

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  • Thin-layer chromatographic developer for detecting residual amount of tripolycyanamide and application of thin-layer chromatographic developer
  • Thin-layer chromatographic developer for detecting residual amount of tripolycyanamide and application of thin-layer chromatographic developer
  • Thin-layer chromatographic developer for detecting residual amount of tripolycyanamide and application of thin-layer chromatographic developer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 The specificity test of coloring agent of the present invention and detection method thereof

[0035] Preparation of the test solution: take by weighing 5.0 g of milk containing an appropriate amount of melamine (or a milk product equivalent to 5.0 g of milk), put it in a stoppered Erlenmeyer flask, add 10 mL of 1% trichloroacetic acid solution, and shake while adding , then add 1mL of 2.2% lead acetate solution and 4mL of chloroform, shake fully for 2min, transfer to a centrifuge tube, and set at 3000r·min -1 Centrifuge for 2 minutes, take the supernatant, put it in the original Erlenmeyer flask, add 10 mL of 1% trichloroacetic acid solution, shake and mix for 2 minutes, transfer the solution to a centrifuge tube, wash the cone with a small amount of 1% trichloroacetic acid solution Shaped bottle, the washing liquid was combined into a centrifuge tube, and the -1 Centrifuge for 2 minutes, and take the supernatant for later use. Transfer the supernatant t...

Embodiment 2

[0039] Embodiment 2 The detection limit test of coloring agent of the present invention and detection method thereof

[0040] Draw the same reference substance solution (0.05mg·mL) of the above-mentioned Example 1 respectively -1 )5, 10μL and reference solution (0.5mg·mL -1 ) 2, 4, and 10 μL were respectively spotted on the same prefabricated silica gel G thin-layer plate, according to the operation of Example 1 "Inspection Method", with acetone-chloroform-ammonia (7:0.5:2, V / V / V) as Developing agent, saturated for 5 minutes, developed, taken out, dried in the air, heated at 105°C for 10 minutes, taken out, immersed in 1% ethanol solution of p-dimethylaminobenzaldehyde hydrochloride (containing 0.3% hydrochloric acid) while hot for 5 to 15 seconds, taken out, Immediately dry it with hot air, and inspect it under ultraviolet light (365nm).

[0041] The result is as figure 2 shown. The spotting amounts of Nos. 1 to 5 in the figure are 0.25, 0.5, 1.0, 2.0 and 5.0 μg in seque...

Embodiment 3

[0042] Embodiment 3 The recovery rate test of colorant of the present invention and detection method thereof

[0043] Weigh 5.0 g of 3 parts of milk without melamine, add different amounts of melamine reference solution respectively, so that the melamine content is 2, 5, 10 mg·kg -1 , and the serial numbers are the test solution ①, the test solution ②, and the test solution ③. Sample preparation in the same manner as in Example 1 "Preparation of the test solution", the concentrations of melamine in the test solution ①, ② and ③ were 0.02, 0.05, 0.10 mg·mL respectively -1 . Draw the reference substance solution (0.5mg·mL -1 ) 2, 4 μL and test solution ① 50, 100 μL, test solution ② 25, 50 μL, test solution ③ 25 μL, respectively spot on the same prefabricated silica gel G thin-layer plate, and operate in the same way as in Example 1 "Inspection method".

[0044] The result is as image 3 As shown, No. 1 to No. 2 in the figure are reference substance solutions, and the sample v...

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Abstract

The invention discloses a thin-layer chromatographic developer for detecting residual amount of tripolycyanamide and application of the thin-layer chromatographic developer. The developer contains 0.1 to 10 weight percent of p-dimethylaminobenzaldehyde and 0.1 to 2 weight percent of ethanol solution of inorganic acid such as hydrochloric acid or sulfuric acid respectively. During detection, a tested sample solution which contains tripolycyanamide and is sufficiently dissolved in a tripolycyanamide organic good solvent with the boiling point of less than or equal to 100 DEG C is applied to a silica gel chromatoplate and developed by the developer in a conventional way and then the developer is volatilized; after a sample is developed by the developer, development spots on the thin-layer chromatoplate are observed under an ultraviolet light or a natural light; and whether the tripolycyanamide content of the tested sample surpasses the prescribed limit is computed according to the amount of the applied sample. By the method, the spots of tripolycyanamide are clear; the detecting sensitivity is high; and the minimum detection value of tripolycyanamide can be 0.5mg.kg<-1>. The method is applicable for detecting the tripolycyanamide content of the food for people and / or animals, including dairy products.

Description

technical field [0001] The invention relates to a thin-layer chromatography color developer for detecting the residual amount of melamine and its application in detecting the residual amount of melamine. Background technique [0002] Melamine is a triazine nitrogen-containing heterocyclic compound, referred to as triamine, also known as melamine, cyanuramide, tripolyamide, etc. It is a white powder that can be dissolved in methanol, formaldehyde, acetic acid, Hot ethylene glycol, glycerin, pyridine, ethanol and other organic solvents and water, insoluble in ether, benzene and carbon tetrachloride, etc. Melamine is a widely used organic chemical raw material and important intermediate, but it is not an additive ingredient allowed in human or animal food. In recent years, there have been incidents of adding melamine to pretend to be protein in a variety of foods including dairy products and livestock and poultry feed, which endangers the health of humans and / or animals. Trig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/90
Inventor 晁若冰王雪彦
Owner SICHUAN UNIV
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