Detection method and application of 2-methylimidazole and 4-methylimidazole in baked food

一种甲基咪唑、检测方法的技术,应用在测量装置、仪器、科学仪器等方向,能够解决未考虑到同分异构体检测的干扰、增大检测工作量和测试成本、薄层色谱法操作步骤多等问题,达到避免目标化合物的损失、降低健康威胁、提高灵敏度的效果

Inactive Publication Date: 2016-04-20
FUJIAN INSPECTION & RES INST FOR PROD QUALITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, thin-layer chromatography has many operational steps and is inaccurate in quantification; spectrophotometry is seriously interfered by the matrix, and the measurement results have large deviations; the sample pretreatment of GC and GC-MS methods is cumbersome and requires derivatization; Susceptible to the interference of impurities, prone to false positives; LC-MS / MS and UPLC-MS / MS methods, sample pretreatment methods mainly include QuEChERS kit, ion pair extraction, solid phase extraction, supercritical fluid extraction, cation exchange Adsorption, etc. Although these purification methods can reduce interference and improve sensitivity, they increase the detection workload and test cost, and the current methods do not take into account the possible interference of the isomer 1-MEI on the detection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0057] Detection of 2-MEI and 4-MEI in commercially available biscuits containing caramel pigment:

[0058] (1) Preparation of standard solution and working curve: prepare a mixed standard solution of 2-MEI and 4-MEI with 20% acetonitrile, and serially dilute to obtain 2-MEI concentrations of 5.3, 10.6, 42.2, 84.4, 105.5, 126.6, 168.8, 266.3 ng / mL, a series of mixed standard solutions with 4-MEI concentrations of 7.1, 14.2, 56.9, 113.7, 142.2, 170.6, 227.4, and 284.3 ng / mL, in which the concentration of 4-MEI-d5 is 88.44 ng / mL. Determination by adding standard method of blank matrix and quantification by internal standard method.

[0059] (2) Preparation of sample solution: Accurately weigh 3.0 g (accurate to 0.01 g) of the pulverized and mixed sample into a 25 mL stoppered colorimetric tube, add 88.44 μg / mL 4-MEI-d525 μL, and then add 10 mL of 5% trichloroacetic acid (containing 20% ​​methanol by volume) solution, vortexed to mix, ultrasonically oscillated for 30min, dilute ...

Embodiment 2

[0081] Detection of 2-MEI and 4-MEI in bread:

[0082] Standard curve making, sample processing and determination are the same as in Example 1. The contents of 2-MEI and 4-MEI in commercially available bread were lower than the detection limit.

Embodiment 3

[0083] Example 3: Detection of 2-MEI and 4-MEI in cookies

[0084] Standard curve making, sample processing and determination are the same as in Example 1. The measured contents of 2-MEI and 4-MEI in commercially available cookies were 11.48 μg / kg and 584.78 μg / kg, respectively.

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Abstract

The invention discloses a detection method of 2-methylimidazole and 4-methylimidazole in baked food. A mixed solution of trichloroacetic acid and methyl alcohol is added to a baked food sample to make protein, colloid and other impurities subside, supersonic extraction is conducted, a solution to be detected is obtained through centrifugation and filtering, a CAPCELL CR (1:4) chromatographic column (5 microns, 2.0 mm*150 mm) is adopted for separation, and the 2-methylimidazole and the 4-methylimidazole are subjected to qualitative and quantitative analysis through an isotope dilution ultra high performance liquid chromatography tandem mass spectrometry method. The method is free of solid phase extraction and other complex sample pre-processing procedures, three types of isomeride of the methylimidazole can be effectively separated, the ion inhibition effect is effectively lowered, sensitivity is improved, and the detection method has the advantages of being low in detection limit and good in accuracy.

Description

technical field [0001] The invention relates to a detection method and application of 2-methylimidazole and 4-methylimidazole in baked food. Background technique [0002] Methylimidazole is a nitrogen-containing heterocyclic compound. Methylimidazoles containing a methyl group include 1-methylimidazole (1-MEI), 2-methylimidazole (2-MEI) and 4-methylimidazole (4 -MEI) three isomers, of which 2-MEI and 4-MEI have a strong convulsive effect, and the US National Toxicology Program (NTP) has proved that 2-MEI and 4-MEI are carcinogenic through animal toxicology experiments , the International Agency for Cancer (IARC) lists it as a Group 2B "probable human carcinogen". The California Office of Environmental Health Risk Assessment (OEHHA) recommends that the daily intake of 4-methylimidazole should be less than 29 μg. The caramel color produced by ammonia method and ammonium sulfite method is the main source of 2-MEI and 4-MEI. The national standard GB8817-2001 of the People's R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 林钦庞美蓉戴明张英郑小严周鹏
Owner FUJIAN INSPECTION & RES INST FOR PROD QUALITY
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