Method for measuring patulin in apple juice

The technology of a patulin and an assay method, which is applied in the field of rapid detection of patulin in apple juice, can solve the problems of complicated operation steps, large amount of reagents, lengthy process and the like, achieves strong specificity, reduces detection limit, Strong anti-interference ability

Inactive Publication Date: 2010-07-21
新疆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

AI Technical Summary

Problems solved by technology

[0004] In view of the shortcomings of the existing methods for the determination of patulin in apple juice, such as lengthy process, cumbersome operation steps, time-consuming, and l

Method used

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  • Method for measuring patulin in apple juice
  • Method for measuring patulin in apple juice

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.3 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed solid-phase extraction column, use a test tube with 30 μL of glacial acetic acid to receive the eluate, and elute with 4 mL of ethyl acetate at 40°C Blow dry slowly with nitrogen gas, add 240 μL of acetonitrile to dissolve, accurately pipette 150 μL of the solution into a 1.5 mL screw-top high-recovery sample bottle, add 50 μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 1 min, and cool , for gas chromatography-mass spectrometry.

Embodiment 2

[0035] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.4 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed-type solid-phase extraction column, use a test tube added with 30 μL of glacial acetic acid to receive the eluate, and elute with 6 mL of ethyl acetate. Blow dry slowly with nitrogen, add 240

[0036] Dissolve in μL of acetonitrile, accurately pipette 150μL of the solution into a 1.5mL screw-top high-recovery sample bottle, add 50μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 3min, cool down, and use for gas chromatography-mass spectrometry determination .

Embodiment 3

[0038] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.7 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed-type solid-phase extraction column, use a test tube added with 30 μL of glacial acetic acid to receive the eluate, and elute with 8 mL of ethyl acetate. Blow dry slowly with nitrogen gas, add 240 μL of acetonitrile to dissolve, accurately pipette 150 μL of the solution into a 1.5 mL screw-top high-recovery sample bottle, add 50 μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 5 minutes, and cool , for gas chromatography-mass spectrometry.

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Abstract

The invention discloses a method for fast measuring patulin in apple juice. The method comprises the following steps: weighing 5.00 grams of apple and shaking the apple in a centrifuge tube; adding 5mL of ethyl acetate-normal hexane solution (95+5, V/V); shaking the centrifuge tube and adding 0.3-0.7 gram of sodium bicarbonate; fiercely shaking the centrifuge tube, carrying out centrifugation, moving 3.2mL of supernate to ethyl acetate activated Crab/C18 mixed type solid phase extraction column, using a test tube with 30mu L of glacial acetic acid to receive eluent, eluting 4-8mL ethyl acetate, injecting nitrogen for drying, adding 240mu L acetonitrile for dissolving, accurately moving 150mu L of solvent to a sample bottle, adding 50mu L of derivatization reagent; using a shock insulator for sealing, carrying out microwave heating for 1-5min, cooling gas phase color spectrum-mass spectrum measurement. The method is a fast, easy and convenient, sensitive, specific durable and quantitative method for confirmation, thus being widely applied to the field where patulin in apple juice is measured.

Description

field of invention [0001] The invention belongs to the field of food safety detection, in particular to a detection method for harmful toxin compounds in food, in particular to the field of a method for rapidly detecting patulin in apple juice. Background technique [0002] Patulin (PAT), also known as patulin. Chemical name: 4-hydroxy-4H-furo(3,2-c)pyran-2(6H)one (4-hydroxy-4H-Furo[3,2-c]Pyran-2(6H)-One) , is a class of toxic compounds belonging to mycotoxins, mainly the secondary metabolites of various fungi such as Penicillium, Aspergillus and Byssochlamys, and has strong antibacterial activity. The cells and tissues of the plant have strong toxicity, and are potentially carcinogenic, teratogenic and mutagenic, and mainly exist in apples, pears and grapes. The EU stipulates that in fruit juice, especially apple juice and alcoholic beverages containing apple juice, the maximum limit of patulin is 50 μg / L, in solid apple products, the maximum limit of patulin is 25 μg / L, ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
Inventor 李锋格姚伟琴窦辉苏敏刘思聪李欣胡建民李炎沈梦园
Owner 新疆出入境检验检疫局检验检疫技术中心
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