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A kind of detection method of dihydropyridine in feed

A dihydropyridine and detection method technology, which is applied in the detection field of dihydropyridine in feed, can solve problems such as unfavorable detection, inconsistent detection results, easy oxidation of dihydropyridine, etc., and achieve low detection limit, high accuracy, advanced Effects with simple processing steps

Active Publication Date: 2020-03-31
HEILONGJIANG PONY TESTING TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention solves the problem that dihydropyridine is easily oxidized, which is not conducive to detection and causes the detection result to be inconsistent with the actual situation, and fills the gap in the accurate determination of the amount of additive dihydropyridine in the feed industry

Method used

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  • A kind of detection method of dihydropyridine in feed
  • A kind of detection method of dihydropyridine in feed
  • A kind of detection method of dihydropyridine in feed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Determination of the content of dihydropyridine in a commercially available 6 different kinds of feeds with different functions

[0043] Each sample was parallelized twice, and the results are shown below.

[0044] Table 1 Dihydropyridine content in feed

[0045]

[0046] ND: not detected

Embodiment 2

[0047] Example 2 The precision determination of dihydropyridine detection method in feed

[0048] Two positive samples were randomly selected, and six parallel determinations were made for each group of samples. The final results are shown below.

[0049] Table 2 Determination of precision

[0050]

Embodiment 3

[0051] Example 3 Determination of accuracy of dihydropyridine detection method in feed

[0052] The negative feed samples that were determined not to contain dihydropyridine were selected for the recovery test of spiked samples as a measure of accuracy. The spiked amounts were 10ng, 25ng, and 50ng respectively. Three parallel experiments were carried out for each spiked sample. The results are shown in the table below.

[0053] Table 3 Addition recovery experiments

[0054]

[0055]

[0056] It can be seen from the measurement that the standard addition recovery rate is between 90.03% and 99.39%, and the relative standard deviation is between 0.43% and 4.80%. Determination of detection limit of dihydropyridine detection method in embodiment 4 feed

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Abstract

The invention belongs to the field of feed detection, and relates to a detection method of diludine in feed. The detection method comprises the following steps: weighing a proper amount of crushed and uniformly mixed feed sample, adding 0.1 mol / L of hydrogen peroxide solution, and standing in a thermostatic water bath; adding acetonitrile, homogenizing by a homogenizer and then centrifuging, evaporating supernatant by a rotary evaporator and then concentrating until the supernatant is nearly dry; fixing the volume with acetonitrile and degreasing with normal hexane, filtering a solution on a lower layer, and measuring by a high performance liquid chromatography-tandem mass spectrometer; carrying out qualitative and quantitative analysis by using qualitative and quantitative ions, wherein a detection limit is 0.001mg / kg. The detection method disclosed by the invention has the characteristics of accurate qualitative analysis, high quantification speed, simple steps, capability of effectively eliminating interference and the like; in addition, the detection method is suitable for detecting the addition amount of the diludine in livestock, poultry and aquatic feed being in a solid state at normal temperature.

Description

technical field [0001] The invention belongs to the field of feed detection, and relates to a detection method of dihydropyridine in feed, in particular to a detection method of hydrogen peroxide oxidation-ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of solid livestock, poultry and aquatic feed at normal temperature Method for the detection of dihydropyridines. Background technique [0002] Diludine (diludine), chemical name is 2,6-dimethyl-3,5-diethylcarboxylate-1,4-dihydropyridine, slightly soluble in water, soluble in hot ethanol, easy to decompose when exposed to light , easy to oxidize, tasteless, non-toxic, melting point 176°C-183°C. Dihydropyridine is a new type of multifunctional feed additive, which has a wide range of biological functions, including promoting the growth of livestock and poultry, improving the quality of livestock and poultry products, improving the reproductive performance of livestock and poultry, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/884
Inventor 宋薇甄玉萍高俊海
Owner HEILONGJIANG PONY TESTING TECH CO LTD
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