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Method for simultaneously detecting two glucocorticoid isomerides in animal-derived food

A technology for glucocorticoids and isomers, applied in the fields of food safety testing and analytical chemistry, can solve the problems of difficult test results, inability to judge mixtures, and high cost

Inactive Publication Date: 2015-07-01
内蒙古出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since betamethasone and dexamethasone, fluorometholone and deoxymethasone are two pairs of epimers, the diastereoisomers that differ only in the configuration of carbon atoms are very similar in chromatographic behavior, Difficult to separate completely
Usually the separation of such isomers requires the use of unconventional chiral chromatographic separation columns, but the cost is high and it is difficult to be widely used
None of the current detection and analysis methods can use conventional chromatographic columns to chromatographically separate the two pairs of isomers, so that when the sample is positive, it is impossible to judge whether it contains a mixture or a single isomer, and it is impossible to confirm which isomer it is , which brings difficulties to the judgment of the test results and easily leads to misjudgment

Method used

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  • Method for simultaneously detecting two glucocorticoid isomerides in animal-derived food
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  • Method for simultaneously detecting two glucocorticoid isomerides in animal-derived food

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Determination of betamethasone, dexamethasone, fluorometholone and deaximethasone in embodiment 1 mutton.

[0042] (1) Sample extraction: Weigh 2.5 g of the mixed sample, add 20 mL of methanol, vortex, shake for 15 min, sonicate for 10 min, centrifuge at 10,000 r / min for 5 min, transfer the supernatant to a rotary steamer, and spin evaporate to near dryness below 40°C. Transfer the liquid in the rotary evaporator to a centrifuge test tube, wash the rotary evaporator with 2ml of methanol, transfer the washing solution to the test tube, dilute to 14ml with water, vortex and mix for 2min, centrifuge at 10000r / min for 5min, and collect the supernatant for use.

[0043] (2) Purification of the extract: install the solid-phase extraction column, activate it with 5ml of methanol and 5ml of water, put the extract on the column, control the flow rate <2ml / min, rinse with 4ml of eluent and 5ml of n-hexane respectively, and use 6 ml of methanol for elution. The eluate was blown d...

Embodiment 2

[0059] Example 2 Determination of betamethasone, dexamethasone, fluorometholone and deoxymethasone in milk.

[0060] (1) Sample extraction: Weigh 5.0 g of the mixed sample, add 20 mL of methanol, vortex, shake for 15 min, sonicate for 10 min, centrifuge at 10,000 r / min for 5 min, remove the supernatant to a rotary evaporator, and rotatable below 40°C until nearly dry. Transfer the liquid in the rotary evaporator to a centrifuge test tube, wash the rotary evaporator with 2ml of methanol, transfer the washing solution to the test tube, dilute to 14ml with water, vortex and mix for 2min, centrifuge at 10000r / min for 5min, and collect the supernatant for use.

[0061](2) Purification of the extract: install the solid-phase extraction column, activate it with 5ml of methanol and 5ml of water, put the extract on the column, control the flow rate <2ml / min, wash it with 4ml of eluent and 5ml of n-hexane respectively, and use 6ml of methanol eluted. The eluate was blown dry with nitro...

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Abstract

The invention discloses a method for simultaneously detecting two glucocorticoid isomerides in animal-derived food. The method separates two enantiomers of betamethasone, dexamethasone, fluorometholone and desoximetasone by adopting a conventional chromatographic column, and can detect the residual amount of betamethasone, dexamethasone, fluorometholone and desoximetasone in the animal-derived food and confirm. A C18 chromatic column is adopted for liquid chromatogram; the flow phases are respectively acetonitrile containing methyl alcohol and water containing methyl alcohol, and tandem mass spectrum detection is carried out; two enantiomers of betamethasone, dexamethasone, fluorometholone and desoximetasone can be subjected to chromatograph separation; the detection limit of dexamethasone is 0.2 micron g / kg; the detection limit of betamethasone, fluorometholone and desoximetasone is 0.4 micron g / kg; the residual amount regulatory restriction requirement at home and abroad is met; the method is simple, convenient, accurate, flexible and reliable.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry and food safety detection, and relates to a liquid chromatography-tandem mass spectrometry detection method for betamethasone, dexamethasone, fluorometholone and deoxymethasone in animal source food, especially for the detection of betamethasone Chromatographic separation and confirmatory analysis of two pairs of isomers with dexamethasone, fluorometholone and deoxymethasone. Background technique [0002] Betamethasone, Dexamethasone, Fluorometholone and Desoxinetasone belong to glucocorticoid veterinary drugs, which are abused and misused in the breeding industry, making some animal sources Residues of such hormonal veterinary drugs will appear in food. Long-term consumption of animal-sourced foods containing glucocorticoid veterinary drugs will affect the hormone balance of the body, which may cause abnormal development in young children and may cause cancer. The maximum residues of glucocor...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 潘国卿郑书展牟峻李刚张春艳白国涛
Owner 内蒙古出入境检验检疫局检验检疫技术中心
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