Sample degreasing method for detecting residues of synthetic hormones in animal-derived food

A technology of sex hormones and animal sources, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of long processing time equipment conditions, loss of target synthetic sex hormones, clogging of solid phase extraction columns, etc., achieve good promotion and application value, and avoid losses , High fat removal efficiency

Inactive Publication Date: 2012-04-18
宁波市产品质量监督检验研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the sample pretreatment methods for the detection of synthetic sex hormone residues in animal foods often use figure 1 steps shown in the figure 1 In the sample pretreatment process shown, degreasing is one of the key technologies for the success of the experiment, because poor degreasing effect will cause blockage of solid phase extraction column and large matrix effect. The commonly used degreasing methods indicated in the figure are as follows Defects: (1) The polarity of many synthetic sex hormones is not very strong for n-hexane degreasing, which leads to the loss of target synthetic sex hormones; (2) Freezing degreasing requires a long processing time and relatively harsh equipment conditions, and the The method is only useful for muscle tissue, but for aquatic products such as fish and egg products such as poultry eggs, there is still the problem of solid-phase extraction column clogging

Method used

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  • Sample degreasing method for detecting residues of synthetic hormones in animal-derived food
  • Sample degreasing method for detecting residues of synthetic hormones in animal-derived food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Sample degreasing method for the detection of synthetic sex hormone residues in fish samples

[0016] 1. Reagents and standard substances used

[0017] Water: ultrapure water

[0018] Methanol: chromatographically pure

[0019] Formic Acid: Superior Pure

[0020] Standard substances: Norgestrel, Methyltestosterone, Testosterone propionate, Medroxyprogesteroue Acetate, Megestrol acetate, Chloridine acetate Progesterone (Chlormadinone acetate), nandrolone (Nandrolone); Ethinylestradiol (Ethinylestradiol); 17α-Estadiol (17α-Estadiol); 17β-Estadiol (17β-Estadiol); -Zeranol); Estrone (Estrone); Dienestrol (Dienestrol); Hexestrol (Hexestrol); Estriol (Estriol); Estradiol- 13 C 2 (Estadiol- 13 C 2 ); Diethylstilbestrol-d 8 ((Diethylstilbestrol) and other standard products were purchased from Dr.Ehrenstorfer GmbH, with a content of ≥98%; Diethylstilbestrol (Diethylstilbestrol) was purchased from Sigma-Aldrich, deuterated nandrolone (Nandrolone-d 3 ) was purc...

Embodiment 2

[0026] Example 2: Sample Degreasing Method for Synthetic Sex Hormone Residue Detection in Egg Products

[0027] 1. Reagents and standard substances used

[0028] With embodiment 1.

[0029] 2. Main instruments and materials

[0030] With embodiment 1.

[0031] 3. Sample pretreatment process

[0032] Weigh 5.0g of the broken salted egg sample, accurate to 0.1g, and place it in a 50mL plastic centrifuge tube with stopper. If it is a spiked sample, add a certain amount of standard solution and internal standard (concentration of internal standard: deuterium deuterium dragon-d 3 , 2μg / kg; Estradiol- 13 C 2 4 μg / kg; diethylstilbestrol-d 8 , 4 μg / kg), then add 10 mL of 0.2 mol / L pH=5 acetic acid-sodium acetate buffer solution, then add 50 μL of β-glucuronidase / arylsulfatase enzymatic hydrolysis solution, and place in a 37°C water bath shaker Shake the enzymatic hydrolysis for 12 hours, take it out and cool to room temperature, add 15mL of methanol, vortex and mix well, ultra...

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Abstract

The invention relates to a sample degreasing method for detecting residues of synthetic hormones in animal-derived food, which is characterized by comprising the following steps: (1) enzymolysis and release of residues of combined type synthetic hormones; (2) extraction of residues of synthetic hormones: adding organic solvents for extracting to obtain supernatant liquid after the enzymolysis reaction is finished; (3) removal of lipids: adding divalent metal hydrochloride in the supernatant liquid for precipitation and centrifugal separation to obtain supernatant liquid; (4) preparation of extract of objective synthetic hormones: evaporating to almost dry the degreased supernatant liquid, adding organic solvents and water, and then, obtaining the extract of objective synthetic hormones; and (5) solid-phase extraction column purification: carrying the extract of objective synthetic hormones into a solid-phase extraction column, collecting the eluent, blow-drying the eluent with nitrogen gas, adding organic solvents for dissolving, using a filter membrane for filtering, and then, testing with a computer. The invention has the advantages of higher degreasing efficiency and simple operation and can avoid the plugging of the solid-phase extraction column and the loss of objective synthetic hormones, thereby obtaining better recovery rate.

Description

technical field [0001] The invention relates to a sample pretreatment method for detection of synthetic sex hormone residues in animal source foods, in particular to a sample degreasing method for detection of synthetic sex hormone residues in animal source foods. Background technique [0002] Synthetic sex hormones are a class of low-molecular-weight, strongly lipophilic, and biologically active steroids secreted by animal gonads or artificially synthesized. Because synthetic sex hormones have the functions of increasing appetite, suppressing estrus, and increasing body weight, and a very small amount can produce a great growth-promoting effect. Therefore, in order to pursue the high economic benefits of animal breeding, producers of animal source food have often used artificially synthesized sex hormones in animal husbandry production since the 1950s. [0003] Synthetic hormones have high stability and remain in food of animal origin. Normal cooking and processing cannot ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/14
Inventor 王全林孙建强沈坚张爱芝
Owner 宁波市产品质量监督检验研究院
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