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Method for simultaneously detecting residue quantities of multiple hormone veterinary drugs

A technology for veterinary drug residues and detection of animals, which is applied in the fields of food safety and analytical chemistry, can solve the problems of lack of gas chromatography-mass spectrometry detection methods for hormone residues, cumbersome operations, etc., and achieve high extraction efficiency, improved efficiency, and simple equipment Effect

Inactive Publication Date: 2012-10-24
林维宣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on gas chromatography-mass spectrometry, and most of the known gas chromatography-mass spectrometry methods are cumbersome to operate, and there is still a lack of mature gas chromatography-mass spectrometry detection methods for hormone residues in animal-derived foods

Method used

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  • Method for simultaneously detecting residue quantities of multiple hormone veterinary drugs
  • Method for simultaneously detecting residue quantities of multiple hormone veterinary drugs
  • Method for simultaneously detecting residue quantities of multiple hormone veterinary drugs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Example 1 Detection method for simultaneous detection of multiple hormone veterinary drug residues in pork

[0074] 1. Sample extraction: Weigh 5g of pork sample into a 50ml plastic centrifuge tube, add 25ml of acetonitrile, homogenize, centrifuge at 4000r / min for 3min, transfer the supernatant into a 125ml separating funnel, and add 15ml of acetonitrile, ultrasonic extraction for 5min, after centrifugation, the supernatant was transferred to the above-mentioned 125ml separatory funnel.

[0075] 2. Degreasing of the extract: Add 25 mL of n-hexane to the extract of the separating funnel, shake for 1 minute, and after standing for stratification, put the acetonitrile layer into another 125 ml separating funnel, then add 25 mL of n-hexane to extract once , after static separation, the acetonitrile layer was transferred to a 100 ml chicken heart bottle, blown dry with a nitrogen blower in a water bath at 40°C, and dissolved with 0.2 mL of methanol.

[0076] 3. Purificati...

Embodiment 2

[0116] Example 2 Detection method for simultaneous detection of multiple hormone veterinary drug residues in pig liver

[0117] 1. Sample extraction: Weigh 5g of pig liver sample into a 50ml plastic centrifuge tube, add 25ml of acetonitrile, homogenize, centrifuge at 4000r / min for 3min, transfer the supernatant into a 125ml separating funnel, and refill the remaining residual sample. Add 15ml of acetonitrile, ultrasonically extract for 5min, and transfer the supernatant to the above-mentioned 125ml separating funnel after centrifugation.

[0118] 2, extract degreasing: with embodiment 1.

[0119] 3. C18 small column purification: the same as in Example 1.

[0120] 4. Silica gel column purification: the same as in Example 1.

[0121] 5. Purification of amino groups: the same as in Example 1.

[0122] 6. Derivatization reaction: the same as in Example 1.

[0123] 7. Gas chromatography-mass spectrometer measurement: with embodiment 1.

[0124] 8. Linear relationship: same ...

Embodiment 3

[0131] Example 3 Detection method for simultaneous detection of multiple hormone veterinary drug residues in pig kidney

[0132] 1. Sample extraction: Weigh 5g of pig kidney sample into a 50ml plastic centrifuge tube, add 25ml of acetonitrile, homogenize, centrifuge at 4000r / min for 3min, transfer the supernatant into a 125ml separating funnel, and refill the remaining residual sample. Add 15ml of acetonitrile, ultrasonically extract for 5min, and transfer the supernatant to the above-mentioned 125ml separating funnel after centrifugation.

[0133] 2, extract degreasing: with embodiment 1.

[0134] 3. C18 small column purification: the same as in Example 1.

[0135] 4. Silica gel column purification: the same as in Example 1.

[0136] 5. Purification of amino groups: the same as in Example 1.

[0137] 6. Derivatization reaction: the same as in Example 1.

[0138] 7. Gas chromatography-mass spectrometer measurement: with embodiment 1.

[0139] 8. Linear relationship: sam...

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Abstract

The present invention relates to the fields of analytical chemistry and food safety, and provides a method for simultaneously detecting residue quantities of multiple hormone veterinary drugs. The method comprises steps of: extracting a sample with acetonitrile; purifying by three SPE columns, including a C18 column, a silica gel column and an amino column; carrying out a microwave assisted derivatization reaction; and using a DB-5MS capillary column (0.25mm *30m *0.25 mum) to separate and detect residue quantities of nine hormone veterinary drugs. Detection limits of the method of the invention on the nine hormone veterinary drugs, including hexestrol, diethylstilbestrol, dienestrol, etiocholanolone, epitestosterone, oestrone, estradiol, ethinyloestradiol and estriol, are 0.1 mug / kg, 0.3 mug / kg, 0.15 mug / kg, 1mug / kg, 0.17 mug / kg, 0.3 mug / kg; 0.4 mug / kg, 0.35 mug / kg and 0.3 mug / kg respectively. The lower limit of detection of the method provided by the invention meets requirements of related domestic and foreign laws and regulations, and technical indicators, such as precision and recovery rate, are in line with the provisions of relevant standards.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and food safety, in particular, it is a method for simultaneously detecting the residues of various hormone veterinary drugs in animal tissues, and especially relates to hexestrol, diethylstilbestrol, hexadiestrol, reduced urine Gas chromatography / mass spectrometry detection method for 9 kinds of veterinary drug residues including testosterone, epitestosterone, estrone, estradiol, ethinyl estradiol, and estriol. Background technique [0002] It has a history of nearly 50 years to apply hormone active substances to the aquaculture industry. Under specific feeding conditions, it can cause animal protein deposition during animal feeding, thereby improving feed conversion rate, increasing lean meat rate, promoting the growth of livestock, poultry and aquatic animals, and promoting the growth rate of 10-40%, which can be quickly Produce significant and direct economic benefits. However, after nea...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N30/08G01N30/06
Inventor 林维宣陈溪董伟峰赵景红
Owner 林维宣
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