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Method for separating roxarsone and its degradation product in broiler manure

A separation method and technology for degradation products are applied in the field of separation of roxarsone and its degradation products in broiler manure, and can solve the problems of low recovery rate of roxarsone, inability to use inorganic phosphate solution, unsatisfactory effect, etc. The effect of high recovery rate, improved recovery rate, and reduced background interference

Inactive Publication Date: 2016-05-04
BEIJING ACADEMY OF AGRICULTURE & FORESTRY SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reported method for detecting roxarsone content, methanol or dipotassium hydrogen phosphate solution was used to extract pig manure and feed samples, and then purified by solid phase extraction column, but phosphate is a non-volatile salt, in order to prevent ion Due to the accumulation of salt crystals in the source, inorganic phosphate solutions cannot be used in mass spectrometry, and other organic extraction solvents are not ideal for the extraction of organic arsine. Among them, the recovery rate of roxarsone is very low, which cannot meet the detection requirements. , the reason may be that roxarsone combines with impurities such as metal ions in fecal samples to form difficult-to-extract substances, so it is imperative to find a method that can efficiently separate and recover roxarsone and its degradation products in broiler manure

Method used

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  • Method for separating roxarsone and its degradation product in broiler manure
  • Method for separating roxarsone and its degradation product in broiler manure
  • Method for separating roxarsone and its degradation product in broiler manure

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1 Roxarsone recovery test in broiler manure sample

[0033] 1) Fecal sample pretreatment:

[0034] Accurately weigh 0.50 g of freeze-dried broiler feces samples into a 50 mL polypropylene centrifuge tube, add 30.0 mL of methanol / water (1:9, v / v) solution, ultrasonicate at room temperature for 30 min, shake continuously, and then After centrifugation for 30 min, 1 mL of the supernatant was purified with a WaterOasisMax solid-phase extraction cartridge.

[0035] 2) Sample concentration and purification:

[0036] Fix the solid-phase extraction cartridge, and activate the solid-phase extraction cartridge with 1.0 mL of methanol and 1.0 mL of ultrapure water. After activation, add 1.0mL extraction supernatant, then wash the column with 1mL eluent (0.05mol / L sodium acetate / methanol, 95:5, v / v, pH adjusted to 7), wash the column with 1mL after rinsing Eluate (formic acid / methanol / water, 5:75:20, v / v, pH adjusted to 2) was eluted at a flow rate of 1.0mL / min, and the ...

Embodiment 2

[0043] The influence of embodiment 2 extracting liquid on extraction rate

[0044] According to the steps of Example 1, broiler feces samples were extracted with different extracts to compare the extraction efficiencies of different extracts. The composition of each extract is shown in Table 2.

[0045] According to the method of Example 1, the broiler feces samples added with 10 μg of roxarsone were extracted with different extracts, the concentration of roxarsone in the extraction supernatant was measured, the extraction rate was calculated, and each sample was repeated five times. The results are shown in Table 3:

[0046] Table 2 Composition of extracts from different experimental groups

[0047]

[0048] Table 3 Effects of different extracts on the extraction rate of samples added with 10 μg roxarsone (ROX)

[0049]

[0050] The results show that the volume ratio of the extraction solution used in the present invention is methanol / water with a volume ratio of 1:9,...

Embodiment 3

[0051] The impact of embodiment 3 eluent on recovery rate

[0052] According to the steps of Example 1, broiler feces samples were extracted with methanol / water at a volume ratio of 1:9, and then 1 mL of the supernatant was purified with a WaterOasisMax solid-phase extraction cartridge to compare eluents with different compositions and pH values The influence on the recovery rate of exogenous roxarsone, the composition and pH value of each eluent are shown in Table 4.

[0053] According to the method of Example 1, the broiler feces samples added with 10 μg of roxarsine were extracted, and then according to the method of Example 1, the extraction supernatant was purified with a solid phase extraction column, and the elution with different compositions and pH values ​​was used. The roxarsone was eluted with liquid, and the concentration of roxarsone in the eluent was measured, and the recovery rate was calculated. Each sample was repeated five times, and the results were shown i...

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Abstract

The invention discloses a method for separating roxarsone and its degradation product in broiler manure. The method comprises 1, carrying out extraction on a manure sample through a methanol-water extraction agent, 2, condensing and purifying the sample through a solid phase extraction column and 3, determining a roxarsone recovery rate of the manure sample through an external standard method. The separation method utilizes the methanol-water extraction agent with a methanol-water volume ratio of 1: 9 to extract roxarsone residues in the manure sample and has a high recovery rate. When the sample is further purified through a solid phase extraction column, a formic acid-methanol-water agent with a formic acid-methanol-water volume ratio of 5: 65-75: 20-30 is used and an eluant with pH of 2 is used so that an ideal recovery rate is guaranteed and polar compound impurities in the sample can be removed and thus background interference in mass spectrum detection is reduced. The recovery rate of the separation method satisfies later detection requirements.

Description

technical field [0001] The invention relates to the field of separation of chemical substances, in particular to a method for separating roxarsone and its degradation products in broiler feces. Background technique [0002] Roxarsone (3-nitro-4-hydroxyphenylarsenic acid, Roxarsone), an organic arsenic (As) compound, is used as an additive in broiler chicken feed due to its antibacterial and growth-promoting effects. Roxarsone is seldom degraded in animals, and most of it is excreted in feces in the form of the original drug, and enters the environment to cause serious local arsenic pollution. Today, with the deteriorating ecological environment, people are paying more and more attention to the degradation and migration of organic arsenic preparations in the environment and the impact on environmental organisms. Roxarsone enters the environment mainly through livestock and poultry manure. However, until now, this process is poorly understood. In order to study the migration...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/40G01N30/02
CPCG01N1/28G01N1/4055G01N1/4077G01N30/02G01N2001/4061G01N2001/4088G01N2001/4094G01N2030/027
Inventor 计峰宋曙辉陈葵黄建国许晓玲
Owner BEIJING ACADEMY OF AGRICULTURE & FORESTRY SCIENCES
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