A method for separating roxarsone and its degradation products in broiler feces

A technology for degradation products and feces is applied in the field of separating roxarsone and its degradation products in broiler feces, and can solve the problems of low recovery rate of roxarsone, unsatisfactory effect, inability to use inorganic phosphate solution, etc. Recovery rate, increase recovery rate, reduce the effect of background interference

Inactive Publication Date: 2018-11-06
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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  • A method for separating roxarsone and its degradation products in broiler feces
  • A method for separating roxarsone and its degradation products in broiler feces
  • A method for separating roxarsone and its degradation products in broiler feces

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Recovery test of roxarsone in broiler manure samples

[0033] 1) Pretreatment of stool samples:

[0034] Accurately weigh 0.50g of freeze-dried broiler feces sample into a 50mL polypropylene centrifuge tube, add 30.0mL of methanol / water (1:9, v / v) solution, ultrasound for 30min at room temperature, shaking constantly, then 13000r / min Centrifuge for 30 min, and take 1 mL of the supernatant for purification with a Water Oasis@Max solid phase extraction cartridge.

[0035] 2) Sample concentration and purification:

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

Embodiment 2

[0043] Example 2 Effect of extraction liquid on extraction rate

[0044] According to the steps of Example 1, different extraction solutions were used to extract broiler manure samples to compare the extraction efficiency of different extraction solutions. The composition of each extraction solution is shown in Table 2.

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

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

[0047]

[0048] Table 3 The effect of different extraction solutions on the extraction rate of 10 μg roxarsone (ROX) samples

[0049]

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

Embodiment 3

[0051] Example 3 Effect of eluate on recovery rate

[0052] Follow the steps in Example 1 to extract broiler manure samples with a volume ratio of 1:9 methanol / water, and then take 1 mL of the supernatant for purification with a Water Oasis@Max solid-phase extraction cartridge, and compare different compositions and pH values. The influence of the eluent on the recovery rate of exogenous roxarsone, the composition and pH value of each eluent are shown in Table 4.

[0053] Follow the method of Example 1 to extract the broiler manure sample with 10 μg of roxarsone added to the external source, and then use the solid phase extraction cartridge to purify the supernatant according to the method of Example 1, using different compositions and pH values ​​for elution The concentration of roxarsone in the eluate was determined and the recovery rate was calculated. Each sample was repeated five times. The results are shown in Table 5:

[0054] Table 4 The composition and pH value of the eluat...

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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 chemical substance separation, in particular to a method for separating roxarsone and its degradation products in broiler manure. Background technique [0002] Roxarsone (3-nitro-4-hydroxyphenylarsenic acid, Roxarsone) is an organic arsenic (As) compound. Because of its antibacterial and growth-promoting effects, it can be used as an additive in broiler feed. Roxarsone is rarely degraded in animals, and is mostly excreted in the feces in the form of the original drug, and enters the environment to cause serious local arsenic pollution. As the ecological environment is deteriorating day by day, 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. After entering the environment, it may pass through organisms. The degraded or non-b...

Claims

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Application Information

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Patent Type & Authority Patents(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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