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Method for detecting contents of olaquindox metabolite and carbadox metabolite in animal muscle tissue and sample pretreatment method thereof

A sample pretreatment and muscle tissue technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex pretreatment steps and long pretreatment time, and achieve the effect of simple steps, shortened time and good repeatability

Inactive Publication Date: 2018-11-30
BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pretreatment method stipulated in GB / T 20746-2006 has multiple steps such as enzymatic hydrolysis, acidification, and SPE purification. The pretreatment takes a long time, and it takes two days to process a sample.
[0005] Aiming at the problem of complex sample pretreatment steps in the detection of olaquindox metabolites and carbadox metabolites, it is urgent to develop a new sample pretreatment method suitable for detecting the content of olaquindox metabolites and carbadox metabolites in animal muscle tissue. Processing methods, especially efficient and sensitive sample pretreatment methods suitable for liquid-mass detection

Method used

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  • Method for detecting contents of olaquindox metabolite and carbadox metabolite in animal muscle tissue and sample pretreatment method thereof
  • Method for detecting contents of olaquindox metabolite and carbadox metabolite in animal muscle tissue and sample pretreatment method thereof
  • Method for detecting contents of olaquindox metabolite and carbadox metabolite in animal muscle tissue and sample pretreatment method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1. Materials and instruments

[0063] 1.1 Materials

[0064] (1) concentrated hydrochloric acid: 14mol / L, analytically pure;

[0065] (2) Sodium chloride: analytically pure;

[0066] (3) Magnesium sulfate anhydrous: analytically pure;

[0067] (4) Ethyl acetate: chromatographically pure;

[0068] (5) Acetonitrile: chromatographically pure;

[0069] (6) Methanol: chromatographically pure;

[0070] (7) Formic acid: 99%, chromatographically pure;

[0071] (8) n-hexane: chromatographically pure;

[0072] (9) Ultrapure water: Class I water in accordance with GB / T6682;

[0073] (10) 3-Methylquinoxaline-2-carboxylic acid, quinoxaline-2-carboxylic acid, 3-methylquinoxaline-2-carboxylic acid-D4, quinoxaline-2-carboxylic acid-D4 Standard substance: purity>99%;

[0074] (11) Preparation of standard stock solution: Accurately weigh an appropriate amount of MQCA and QCA standard substances, dissolve and constant volume with methanol, and make 100 μg / mL standard stock soluti...

Embodiment 2

[0152] The sample to be tested described in this embodiment is a pork positive sample, which is detected by the following steps:

[0153] (a) Pretreatment of samples, including the following steps:

[0154] Weigh 5g of pork positive sample, put it in a 50mL centrifuge tube, add 100μL of 1μg / mL MQCA-D 4 and QCA-D 4For internal standard solution, add 8mL of 1mol / L hydrochloric acid solution, vortex for 1min, let stand for 30min, then add 10mL of ethyl acetate, vortex for 1min, add 3g of anhydrous magnesium sulfate, 0.5g of sodium chloride, vortex for 1min, centrifuge at 8000rpm for 8min. Take the supernatant in a test tube, blow it dry with nitrogen, make it to volume with 1mL methanol-water-formic acid (1:9:0.001), degrease with methanol-saturated n-hexane, filter through a 0.2μm filter membrane, and perform ultra-high performance liquid chromatography- Triple quadrupole tandem mass spectrometry detection.

[0155] (b) Using ultra-high performance liquid chromatography-tripl...

Embodiment 3

[0157] Verification of embodiment 3 detection method

[0158] 1. Linear range

[0159] In the linear range of 1.0ng / mL to 100ng / ml, the peak area of ​​the target compound is used to make a standard curve for its corresponding mass concentration, and its correlation coefficient (r 2 ) are greater than 0.99, indicating that MQCA and QCA have a good linear relationship in the range of 1.0-100ng / ml.

[0160] 2. The lowest detection limit and the lowest quantification limit

[0161] Referring to the detection limit of 3-methylquinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid in GB / T 20746-2006 is 0.5μg / kg, add 0.5μg / kg target to the blank sample Compounds, the signal-to-noise ratios actually obtained in the test were 35.2 and 25.8, which fully met the hygienic limit requirements. Therefore, the method detection limit of this method was set at 0.5 μg / kg.

[0162] 3. Accuracy and precision

[0163] Pork, beef, chicken, fish, etc. were used as substrates to investig...

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Abstract

The invention discloses a method for detecting contents of olaquindox metabolite and carbadox metabolite in animal muscle tissue and a sample pretreatment method thereof. The sample pretreatment method for detecting the contents of the olaquindox metabolite and the carbadox metabolite in the animal muscle tissue includes the steps that to-be-detected animal muscle tissue samples are taken, hydrochloric acid solution is added for acidolysis, then ethyl acetate is added to extract the olaquindox metabolite and the carbadox metabolite, and mixed liquor is obtained; MgSO4 and Nacl are added to themixed liquor, the vortex and centrifugation are carried out, and supernatant is collected from the upper layer; the supernatant is concentrated and redissolved, then methanol saturation normal hexanesolution is added, the vortex and centrifugation are carried out, the lower solution is collected, the filtration is carried out, and to-be-detected solution is obtained. The invention further discloses the method for detecting the contents of the olaquindox metabolite and the carbadox metabolite by LC-MS after sample pretreatment. The method for detecting the contents of the olaquindox metabolite and the carbadox metabolite in the animal muscle tissue and the sample pretreatment method thereof has short time consumption, easy procedure, good repeatability and high result accuracy.

Description

technical field [0001] The invention relates to the field of food detection. More specifically, it relates to a method for detecting the content of olaquindox metabolites and carbadox metabolites in animal tissue and animal muscle tissue and a sample pretreatment method thereof. Background technique [0002] Quinoxaline drugs are a class of chemically synthesized antimicrobial growth-promoting agents, mainly including olaquindox, carbadox, quinketene, acetylmethaquine and other drugs. Since the eighties in 20th century, quinoxaline drugs have been widely used as a kind of ideal feed additive in the feed of livestock and poultry etc. After animals use quinoxaline drugs, the conversion efficiency of feed can be improved, the assimilation rate of protein can be accelerated, the nitrogen storage content in the animal body can be higher, the cell formation is accelerated, the tissue in the body is enlarged, and the meat growth rate is accelerated. However, excessive use of such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/045G01N2030/062G01N2030/8809
Inventor 严华崔凤云李建辉张朝晖韩深何悦齐鹤鸣
Owner BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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