Method used for detecting Roxarsone and degradation products of Roxarsone in broiler manure

A detection method and technology for degradation products, applied in the field of chemical analysis and detection, can solve problems such as imperfect detection methods and unclear degradation pathways, and achieve the effects of improving recovery rate and reducing background interference.

Inactive Publication Date: 2016-03-02
BEIJING ACADEMY OF AGRICULTURE & FORESTRY SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the imperfect detection method, the degradation pathway of roxarsone after it enters the environment through feces is still unclear

Method used

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  • Method used for detecting Roxarsone and degradation products of Roxarsone in broiler manure
  • Method used for detecting Roxarsone and degradation products of Roxarsone in broiler manure
  • Method used for detecting Roxarsone and degradation products of Roxarsone in broiler manure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 Roxarsone recovery test in broiler manure sample

[0034] 1) Fecal sample pretreatment:

[0035] 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 used for purification with a WaterOasis@Max solid-phase extraction cartridge.

[0036] 2) Sample concentration and purification:

[0037] 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 / m...

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 WaterOasis@Max solid-phase extraction cartridges to compare the different compositions and pH values ​​of the washes. The influence of eluent 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 re...

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Abstract

The invention discloses a method used for detecting Roxarsone and degradation products of Roxarsone in broiler manure. The method comprises following steps: 1) methanol / water is taken as an extracting solution to extract manure samples; 2) a solid phase extraction column is used for further concentration and purification of the samples; and 3) a high performance liquid chromatography-ion trap-time of flight mass spectrometer is used for analysis. According to the method, a pretreatment method of the manure samples is optimized firstly, and the recovery rate of Roxarsone and the degradation products of Roxarsone in broiler manure of the method is capable of satisfying requirements of subsequent detection. The ion trap-time of flight mass spectrometer is used for detecting the samples obtained via pretreatment, accurate mass resolution ratio and sensitivity are improved greatly compared with that of other mass spectrum methods, molecule mass information can be provided accurately, reliability of determined molecular formulas is improved, and the method is useful in identification of organic compounds.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a method for speciation analysis and detection of organic arsenic in animal excrement. 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 migra...

Claims

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Application Information

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IPC IPC(8): G01N30/02
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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