CN1281949C - Method for quickly detecting 4-methyl iminazole in food - Google Patents
Method for quickly detecting 4-methyl iminazole in food Download PDFInfo
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- CN1281949C CN1281949C CN 200410004506 CN200410004506A CN1281949C CN 1281949 C CN1281949 C CN 1281949C CN 200410004506 CN200410004506 CN 200410004506 CN 200410004506 A CN200410004506 A CN 200410004506A CN 1281949 C CN1281949 C CN 1281949C
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Abstract
The present invention discloses a method for quickly detecting 4-methylimidazole in food, which belongs to the detection range of food additives. The method comprises the following principles: the solid-phase extraction to a sample containing caramel pigment is carried out by a solid-phase extraction column (XTR>500 mg); after passing through the column, the sample is eluted by an organic solvent; after the eluent is concentrated, a micro sample applicator is used to directly carry out sample application on a polyamide film used as a chromatographic material; ascending development is carried out in a developing agent with a corresponding proportion; the polyamide film is directly observed with naked eyes after color development in iodine steam. If brown spots with rf values identical to that of a standard sample in a rf value range between 0.5 and 0.7, the detected material contains 4-methylimidazole. The present invention is capable of quickly and qualitatively detecting if a sample is naturally brewed or manually compounded, and is especially suitable for the detection of samples containing caramel pigment, such as soya sauce, vinegar, cola, etc. A developed thin-layer plate can be stored for a long time for reexamination, and a thin-layer scanner can be used for quantitative measurement.
Description
Technical field
The invention belongs to the sensing range of food additives, particularly relate to a kind of method that detects 4-methylimidazole in the food that food production factory detects caramel colorant and contains the food of caramel colorant that can be used as.
Background technology
Caramel colorant is a widely used food colour in a kind of world wide, and about 200,000 tons of the annual consumption in the whole world wherein is used in the Food ﹠ Drink more than 90%.The caramel colorant of the U.S. about 95% is used for beverage; The caramel colorant in Asia is mainly used in soy sauce and other flavouring.For example soy sauce is an indispensable traditional condiment in China's people's lives, along with the raising of living standards of the people, except that requiring soy sauce to have the certain nutritional labeling and organoleptic quality, is had higher requirement in the safety and sanitation aspect of soy sauce.Color and luster is one of important index in the sense index of soy sauce, the color and luster of soy sauce mainly comes from the melanin that produces in the sweat, some comes from the caramel colorant of interpolation, when some factories do not reach the colourity requirement at brewage process, often adds excessive caramel colorant." soy sauce " of some illegal producers with " hair water " and caramel colorant preparation also appearred in the market.
The caramel colorant that is used for soy sauce, vinegar, beverage can produce a certain amount of objectionable impurities 4-methylimidazole in process of production mainly with ammonia process production, experiment showed, the LD of 4-methylimidazole to mouse through animal toxicology
50Value is the 370mg/kg body weight, can cause convulsions even bring out epilepsy, and the content of 4-methylimidazole can not surpass 0.02% in the caramel colorant that standard GB 8817-2001 regulation ammonia (ammonium) method is produced.No matter be the caramel colorant of excessive interpolation in required legal interpolation of production technology or the artificial formulated product, wherein contained 4-methylimidazole all may work the mischief because of long-term the absorption, thereby the content of fast, accurately measuring 4-methylimidazole in the food is very necessary, can be used as quality testing department simultaneously and judges one of index of soy sauce safety.
The assay method of 4-methylimidazole has silicon thin-layer chromatography, paper chromatography, vapor-phase chromatography, the chromatography of ions, high performance liquid chromatography, capillary isotachophoresis method etc. in the caramel colorant at present.The progress along with analytical instrument has reached certain level though the qualitative and quantitative analysis method of caramel colorant is at aspects such as accuracy, precision, and instrument analytical method needs special analytical instrument and expensive testing expense.The problem that silica gel thin-layer chromatography and ply of paper are analysed the method existence of measuring contained 4-methylimidazole in the caramel colorant is to detect limit for height, and sensitivity is low, is difficult to quantitatively, is unsuitable for the micro-4-methylimidazole that contains in the food that adds caramel colorant is detected.
At present, add 4-methylimidazole that caramel colorant brings in the food, separation and purification difficulty and lack special detection method then because of component in the food is many.Particularly at life common foods such as soy sauce, vinegar, the 4-methylimidazole content that detects wherein is one of method of differentiating its security.Therefore it is very necessary to study quick, easy, inexpensive analytical approach.This research provides the technology of discerning brewage and artificial synthetic food aspect the food quality monitoring, provides rapid analysis for strengthening the food products market supervision.
Summary of the invention
The purpose of this invention is to provide a kind of method that detects 4-methylimidazole in the food.It is characterized in that: the step of this method is: be that the sample that will contain caramel colorant obtains analytic sample through the solid-phase extraction column separation and Extraction of XTR＞500mg, after sample is crossed post, with organic solvent wash-out 4-methylimidazole potpourri, use directly point sample 3～6 μ l on the chromatographic material polyamide film of micro-sampling device after the measured object solution concentration, vertically put into airtight, ascending development in the expansion cylinder of developping agent is housed, stop chromatography during apart from film top 0.5～1cm at solvent front, volatilize solvent, by the stifling colour developing of iodine vapor 60 minutes, naked eyes Direct observation behind the iodo steam displaing color, if between Rf value 0.5～0.7, observe the brown spot identical simultaneously, then think and contain 4-methylimidazole in this measured object with the standard specimen Rf value.
Described organic solvent is ethyl acetate or methylene chloride.
Described developping agent is the cyclohexane of proportioning by volume: acetone: ethanol=4～5.5: 0.8～1.2: 0.5～0.9 potpourri
The invention has the beneficial effects as follows and propose to use the measurement in chromatography material of polyamide film first as 4-methylimidazole, this material conveniently is easy to get, launch rapidly, the thin layer plate after the expansion can long preservation be prepared against check, and can use thin-layer chromatogram scanner and carry out quantitative measurement; Utilize the developping agent of suitable proportioning, fully separate targets compound and other component that is dissolved in ethyl acetate or methylene chloride.Therefore this method can realize fast qualitative, detection by quantitative to 4-methylimidazole, be used for overall process that 4-methylimidazole detects and be about 1～2 hour and promptly can obtain the result, and that instrumental analysis takes is longer; Therefore evidence soy sauce, vinegar do not produce 4-methylimidazole in the brew process, can judge that for the detection by quantitative of 4-methylimidazole this product is natural brewages or by manually converting system by the polyamide thin-layer chromatography.Detect cheap: qualitative detection of the present invention partly need not the main equipment expense and drops into, and is easy to promote the use of in basic unit, and simple to operate when particularly whether having a large amount of 4-methylimidazoles as food liquids such as qualitative determination soy sauce, the consumables price is comparatively cheap; Highly sensitive: this method can detect the 4-methylimidazole (in soy sauce 4-methylimidazole content be about 20 μ g/Ls more than) of content greater than 10 μ g/L.
Embodiment
The invention provides a kind of method that detects 4-methylimidazole in the food.This method is to contain the sample of caramel colorant, add behind the filtering with microporous membrane in the solid-phase extraction column through pre-treatment and activation XTR＞500mg, after sample is crossed post, with organic solvent ethyl acetate or methylene chloride wash-out 4-methylimidazole potpourri, use directly point sample 3～6 μ l on the chromatographic material polyamide film of 2 * 8cm of micro-sampling device after the measured object solution concentration, vertically put into airtight, the developping agent cyclohexane of proportioning by volume is housed: acetone: ethanol=(4～5.5): 0.8～1.2: the potpourri of (0.5～0.9) ascending development in expansion cylinder, stop chromatography during apart from film top 0.5～1cm at solvent front, volatilize solvent, about 6.5～the 7cm of development distance, can realize target compound and separated from impurities, by the stifling colour developing of iodine vapor 60 minutes, naked eyes Direct observation behind the iodo steam displaing color, if between Rf value 0.5～0.7, observe the Rf value brown spot identical simultaneously with standard specimen, think then and contain 4-methylimidazole in this measured object that promptly overall process is about 1～2 hour and can obtains the result.The sample that is particularly suitable for soy sauce, vinegar, cola etc. are contained caramel colorant detects.Instrumental analysis takes longer.Also available standard specimen series concentration counter point is realized half-quantitative detection, and also available thin layer chromatography scanning is realized quantitative measurement.
For embodiment the present invention is further specified again below.
Embodiment
Soy sauce 1～the 5mL that contains caramel colorant, add XTR1000mg solid-phase extraction column behind the filtering with microporous membrane through pre-treatment and activation, with organic solvent ethyl acetate or methylene chloride wash-out 4-methylimidazole potpourri, gained measured object solution is direct point sample after concentrating.
With micro-sampling device point sample 3～6 μ L on the polyamide thin plate of 2 * 8cm, vertically put into airtight, developping agent (cyclohexane: acetone: ascending development in expansion cylinder ethanol=5: 1: 0.7) is housed, development distance is 7～7.5cm, compare with quantitative 4-methylimidazole standard items in same thin layer plate, can judge whether target compound exists in this soy sauce, and target compound separates fully under this chromatographic condition with impurity.Take out thin plate, volatilize solvent, iodo steam displaing color, carry out qualitative detection with standard specimen contrast, Direct observation with the naked eye is if observe the Rf value brown spot identical with standard specimen simultaneously between Rf value 0.6～0.7, then think and contain 4-methylimidazole in this measured object, being the soy sauce by artificial preparation that adds caramel colorant, if observe with standard specimen on the contrary identical brown spot not arranged, then is the natural soy sauce of brewageing.Also available standard specimen series concentration counter point is realized half-quantitative detection, and also available thin layer chromatography scanning is realized quantitative measurement.
It should be noted last that the measuring principle of vinegar and cola and method and soy sauce are identical, this patent does not exemplify one by one.
Claims (1)
1. method that detects 4-methylimidazole in the food, it is characterized in that: the step of this method is: be that the sample that will contain caramel colorant obtains analytic sample through the solid-phase extraction column separation and Extraction of XTR＞500mg, after sample is crossed post, with organic solvent ethyl acetate or methylene chloride wash-out 4-methylimidazole potpourri, after the measured object solution concentration, with direct point sample 3～6 μ l on the chromatographic material polyamide film of micro-sampling device, vertically put into airtight, the cyclohexane of proportioning by volume is housed: acetone: ethanol=4～5.5: 0.8～1.2: 0.5～0.9 potpourri is an ascending development in the expansion cylinder of developping agent, stop chromatography during apart from film top 0.5～1cm at solvent front, volatilize solvent, by the stifling colour developing of iodine vapor 60 minutes, naked eyes Direct observation behind the iodo steam displaing color, if between Rf value 0.5～0.7, observe the brown spot identical simultaneously, then think and contain 4-methylimidazole in this measured object with the standard specimen Rf value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410004506 CN1281949C (en) | 2004-02-19 | 2004-02-19 | Method for quickly detecting 4-methyl iminazole in food |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410004506 CN1281949C (en) | 2004-02-19 | 2004-02-19 | Method for quickly detecting 4-methyl iminazole in food |
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| CN1560629A CN1560629A (en) | 2005-01-05 |
| CN1281949C true CN1281949C (en) | 2006-10-25 |
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| CN 200410004506 Expired - Fee Related CN1281949C (en) | 2004-02-19 | 2004-02-19 | Method for quickly detecting 4-methyl iminazole in food |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100350244C (en) * | 2005-10-19 | 2007-11-21 | 大连轻工业学院 | Thin-layer chromatography assay method for Fumonisins B1 |
| CN102062768A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Method for quickly detecting 4-methylimidazole in food |
| CN102590409B (en) * | 2012-01-12 | 2014-05-07 | 广州市质量监督检测研究院 | Method for measuring content of caramel pigments in foods |
| CN104359989A (en) * | 2014-11-07 | 2015-02-18 | 江苏省疾病预防控制中心 | Liquid chromatography detecting method for 2,4-methylimidazole and 2-acetyl-4-tetrahydroxyl-buthylimidazole in caramel pigment |
| CN104833744A (en) * | 2015-06-05 | 2015-08-12 | 上海浩登材料科技有限公司 | Detection method for 4-methylimidazole in food |
| CN110082463A (en) * | 2019-04-30 | 2019-08-02 | 烟台欣和企业食品有限公司 | The detection method of 4-methylimidazole in flavouring |
| CN111735885B (en) * | 2020-08-11 | 2022-06-17 | 浙江省疾病预防控制中心 | Method for pretreatment of tea and/or coffee and simultaneous determination of 1-methylimidazole, 2-methylimidazole and 4-methylimidazole |
| CN113899906B (en) * | 2021-06-17 | 2023-04-07 | 黄埔海关技术中心 | Wine caramel pigment detection robot and detection method |
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