Method for measuring patulin in fruit jam and vegetable paste

A technology for the determination of patulin and its method is applied in the field of rapid detection of patulin in fruit and vegetable sauces, which can solve the problems of cumbersome operation steps, large amount of reagents, and lengthy process, and achieve improved extraction efficiency, short processing time, and specialized strong effect

Inactive Publication Date: 2010-07-14
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

[0005] In view of the shortcomings of the existing method for the determination of patulin, such as lengthy process, cumbersome operation steps, time-consuming, and large amount of reagents, there is no fast, simple, high-sensitivity, accurate, specific, and durable method for the determination of Aspergillus patulin in fruit and vegetable sauces. prime method reports

Method used

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  • Method for measuring patulin in fruit jam and vegetable paste
  • Method for measuring patulin in fruit jam and vegetable paste
  • Method for measuring patulin in fruit jam and vegetable paste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 2.00 grams of fruit and vegetable sauce into a centrifuge tube, add 0.5-3 mL of water, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, and add 0.5-2 grams of sea sand at the same time, 4 -8 grams of anhydrous sodium sulfate and 0.5-2 grams of sodium bicarbonate, shake vigorously for 2 minutes, centrifuge for 3 minutes; use 5 mL of ethyl acetate to activate a carbon black (Carb) solid phase extraction column, pipette 4 mL of supernatant to the carbon black small For the column, use a test tube with 30 μL of glacial acetic acid to receive the eluent, elute with 3-7 mL of ethyl acetate; blow dry slowly with nitrogen gas at 40 ° C, add 240 μL of acetonitrile to dissolve, and accurately pipette 150 μL of the solution to the sample bottle Add 50 μL of derivatization reagent, seal with a septum, react for 1-7min under high-grade microwave conditions of 800W, cool down, and use for gas chromatography-mass spectrometry.

Embodiment 2

[0049] Weigh 2.00 grams of tomato paste into a centrifuge tube, add 3 mL of water, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 1 gram of sea sand, 5 grams of anhydrous sulfuric acid Sodium and 1 g of sodium bicarbonate, shake vigorously for 2 min, and centrifuge for 3 min; activate a carbon black (Carb) solid-phase extraction column with 5 mL of ethyl acetate, transfer 4 mL of the supernatant to a small carbon black column, and add 30 μL of glacial acetic acid The test tube in the test tube received the eluent, and was eluted with 4 mL of ethyl acetate; blown dry slowly under nitrogen gas at 40°C, added 240 μL of acetonitrile to dissolve, accurately pipetted 150 μL of the solution into the sample bottle, added 50 μL of derivatization reagent, and used a septum Gasket sealed, reacted under microwave 800W high-grade condition for 3 minutes, cooled, and used for gas chromatography-mass spectrometry.

Embodiment 3

[0051] Weigh 2.00 grams of apricot jam into a centrifuge tube, add 3 mL of water, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 1 gram of sea sand, 5 grams of anhydrous sulfuric acid Sodium and 1 g of sodium bicarbonate, shake vigorously for 2 min, and centrifuge for 3 min; activate a carbon black (Carb) solid-phase extraction column with 5 mL of ethyl acetate, transfer 4 mL of the supernatant to a small carbon black column, and add 30 μL of glacial acetic acid The test tube in the test tube received the eluent, and was eluted with 4 mL of ethyl acetate; blown dry slowly under nitrogen gas at 40°C, added 240 μL of acetonitrile to dissolve, accurately pipetted 150 μL of the solution into the sample bottle, added 50 μL of derivatization reagent, and used a septum Gasket sealed, reacted under microwave 800W high-grade condition for 3 minutes, cooled, and used for gas chromatography-mass spectrometry.

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Abstract

The invention discloses a method for rapidly measuring patulin in fruit jam and vegetable paste, comprising the following steps: weighing 2.00g of fruit jam and vegetable paste in a centrifuge tube, adding 0.5-3mL of water, shaking, adding 5mL of ethyl acetate-normal hexane solution (95+5, v/v), shaking, simultaneously adding 0.5-2g of sea sands, 4-8g of anhydrous sodium sulfate and 0.5-2g of sodium bicarbonate, shaking vigorously for 2min, and centrifuging for 3min; and weighing 4mL of supernate until ethyl acetate activates a carbon black columella, receipting eluent by a test tube in which glacial acetic acid is added, eluting by 3-7mL of ethyl acetate, and drying; dissolving 240 mu L of acetonitrile, pipetting 150 mu L of dissolution liquid into a sample bottle, adding 50 mu L of derivatization reagent, heating by microwave for 1-7min, cooling and then measuring by gas chromatography-mass spectrometry. The method is rapid, simple, sensitive, accurate, specific and durable in confirmation and quantification, and is widely applied to the measurement filed of patulin in fruit jam and vegetable paste.

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 rapid detection method for patulin in fruit and vegetable sauces. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李锋格姚伟琴田延河苏敏朱慧萍李炎胡建民李欣沈梦园
Owner 新疆出入境检验检疫局检验检疫技术中心
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