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

A technology of methylimidazole and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the interference that does not take into account the detection of isomers, increase the detection workload and test cost, thin-layer chromatography Avoiding the loss of target compounds, reducing health threats, and improving sensitivity due to many operating steps

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,

Method used

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

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0056] Example 1

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

[0058] (1) Preparation of standard solution and working curve: prepare a mixed standard solution of 2-MEI and 4-MEI with 20% acetonitrile, and dilute step by step 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 4-MEI-d5 concentrations were all 88.44 ng / mL. The blank matrix was used for determination, and the internal standard method was used for quantification.

[0059] (2) Preparation of sample solution: Accurately weigh 3.0g (accurate to 0.01g) of the crushed and mixed sample into a 25mL colorimetric tube with a stopper, add 88.44μg / mL 4-MEI-d525μL, and then add 10mL mass percentage of 5% trichloroacetic acid (containing 20% ​​methanol by volume) solution, vortex and shake to ...

Example Embodiment

[0080] Example 2

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

[0082] The standard curve preparation, sample processing and determination were the same as those in Example 1. The levels of 2-MEI and 4-MEI in commercial bread were both below the detection limit.

Example Embodiment

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

[0084] The standard curve preparation, sample processing and determination were the same as those in Example 1. The contents of 2-MEI and 4-MEI in the commercially available cookies were measured to be 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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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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