CN101598711A - The assay method of illegally added industrial dye-acid orange II content in a kind of food - Google Patents
The assay method of illegally added industrial dye-acid orange II content in a kind of food Download PDFInfo
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- CN101598711A CN101598711A CNA2009100868600A CN200910086860A CN101598711A CN 101598711 A CN101598711 A CN 101598711A CN A2009100868600 A CNA2009100868600 A CN A2009100868600A CN 200910086860 A CN200910086860 A CN 200910086860A CN 101598711 A CN101598711 A CN 101598711A
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Abstract
The present invention relates to a kind of method of using the series connection liquid phase mass spectrograph to measure illegally added industrial dye-acid orange II content in the food.By centrifugal and ultrasonic Extraction to sample, getting supernatant adopts Solid-Phase Extraction to purify, inject liquid chromatography-tandem mass spectrometry after crossing 0.22 μ m filter membrane, by carrying out qualitative with (characteristic ion right/quota ion to) pairing LC-MS/MS chromatographic peak area relative abundance of retention time and two pairs of ions to target compound.Require the retention time of target compound in the tested sample consistent with the retention time of target compound in the standard solution, deviation is less than 20%, require simultaneously two pairs of ion pairs of target compound in the tested sample answer the LC-MS/MS chromatographic peak area than with standard solution in the area of target compound than consistent, quantitative measurement.
Description
Technical field
The present invention relates to illegally added industrial dye-acid orange II Determination on content method in a kind of food, particularly relate to a kind of method of using the series connection liquid phase mass spectrograph to measure the content of illegally added industrial dye-acid orange II in the food
Background technology
Acid Orange II is the acid industrial dye of a kind of azo class, has another name called acid golden yellow II, gold orange II or acid gorgeous orange GR, the golden yellow powder of popular name.Water-soluble, ethanol.Be mainly used in the dyeing of silk, wool.Also can dye leather, paper, polyamide fibre.Can stamp.Also can be used as indicator.Discharge, good level-dyeing property, dyefastness is relatively poor, is applicable to the knitting wool dyeing that colour brightness is high.It is red dark to meet the copper ion trend during dyeing, and chance ferric ion lighter color is dark.
The non-food coloring Acid Orange II has another name called gold orange II, No. two oranges, orange orange, acid golden yellow II or acid gorgeous orange GR, the golden yellow powder of popular name, and chemistry beta naphthal azo P-TOLUENE SULFO ACID 99 sodium by name is acid base indicator.Medically be used for tissue section strain, in weaving, be used as the dyeing of colorant, leather and fur products, plastics and woodwork.Acid Orange II is the carcinogenic compound of moderate toxicity, forbids using in food.
Acid Orange II belongs to non-food coloring, does not allow in the food to add.But because Acid Orange II lovely luster, characteristics such as coloring stabilized, inexpensive, some illegal retailers use it for food production and processing in order to seek exorbitant profit, serious harm the consumer healthy.Therefore, promptly and accurately judge whether there is this non-food coloring in the food, setting up one, to overlap the assay method of non-food coloring Acid Orange II in the food fast and accurately significant.
Summary of the invention
The present invention is to provide illegally added industrial dye-acid orange II Determination on content method in a kind of food.
1 principle
Target compound in the sample extracts with methyl alcohol-ammonium acetate solution, behind weak anionic exchange Solid-Phase Extraction column purification, and liquid chromatography tandom mass spectrometry determination, matrix mark-on working curve external standard method is quantitative.
2 reagent and material
Except as otherwise herein provided, it is pure that all reagent are analysis, and experimental water is a ultrapure water.
2.1 methyl alcohol: liquid chromatography is pure
2.2 ammonium acetate
2.3 formic acid
2.4 ammoniacal liquor
2.5 extraction solution: take by weighing 3.9 gram ammonium acetate water dissolvings, add 10.0mL formic acid, the water constant volume arrives 1000mL with methanol constant volume behind 500mL.
2.6 solid-phase extraction column balance solution: take by weighing 3.9 gram ammonium acetate water dissolvings, add 10.0mL formic acid, the water constant volume is to 500mL.
2.7 eluent solution: take by weighing 3.9 gram ammonium acetate water dissolvings, add 10.0mL formic acid and 25.0mL methyl alcohol, the water constant volume is to 500mL.
2.8 elute soln: get 5mL ammoniacal liquor with methanol constant volume to 100mL.
2.9 sample diluting liquid: take by weighing 0.39 gram ammonium acetate water dissolving, add 0.50mL formic acid, the water constant volume is behind 250mL, and the water constant volume is to 500mL.
2.10 mobile phase A: take by weighing 0.39 gram ammonium acetate water dissolving, add 0.50mL formic acid, the water constant volume is to 500mL.
2.11 Mobile phase B: acetonitrile, liquid chromatography is pure.
2.12 weak anionic exchange solid-phase extraction column: WAX, 60mg/3mL uses 3mL methyl alcohol, 3mL water and 3mL solid-phase extraction column balance solution (2.5) activation successively before the use.
2.13 standard items: Acid Orange II.
2.14 standard reserving solution (1.0mg/mL): accurately take by weighing 0.0100 gram Acid Orange II standard items, be settled to 10.0mL with 50% methanol aqueous solution.
25,50,100,200,400ng/mL 2.15 standard series: preparation Acid Orange II standard series, Acid Orange II concentration is:.
3 instrument and equipments
3.1 liquid chromatography-tandem mass spectrometry instrument: be furnished with electron spray (ESI) ion gun.
3.2 hydro-extractor.
3.3 ultrasound bath.
3.4 solid-phase extraction device.
3.5 Nitrogen evaporator.
The preparation of 4 samples and matrix mark-on working curve
4.1 the preparation of sample
A) extract
Take by weighing 1.0 gram samples in the 50mL centrifuge tube, add 10.0mL and extract solution, ultrasonic Extraction 30 minutes, centrifugal 10 minutes of 10000r/min, supernatant are transferred in another 50mL centrifuge tube; Add 10.0mL extraction solution in the residue and extract once more, merge extracted twice solution.
B) purify
Get the 5.0mL sample extracting solution, be settled to 50.0mL with solid-phase extraction column balance solution (2.5) dilution, cross the weak anionic solid-phase extraction column that has activated, with 2mL leacheate, 2mL water wash, 5mL eluent wash-out is collected eluent, blows near with nitrogen and does, be settled to 1.0mL with sample diluting liquid, excessively liquid chromatography tandom mass spectrometry determination behind the 0.22 μ m filter membrane.
4.2 the preparation of matrix mark-on working curve
Take by weighing 1.0 gram blank sample matrix in the 50mL centrifuge tube, take by weighing 6 parts, add standard serial solution (2.15) 100 μ L respectively, operate by 4.1, preparation matrix mark-on working curve, 25,50,100,200,400ng/mL Acid Orange II is:.。
5 measure
5.1 liquid chromatography-tandem mass spectrometry reference conditions
Chromatographic column: BHT 1.7 μ m * 100mm
Moving phase: the 5mmol/L ammonium acetate of 0.1% formic acid is water-soluble+acetonitrile 9 (1+9).
Sample size: 5 μ L.
Column temperature: 40 ℃.
Ion gun: Acid Orange II electron spray ESI, negative ion.
Scan mode: multiple-reaction monitoring MRM.
The monitoring ion pair:
| Component | Taper hole voltage (v) | Collision energy (ev) | Parent ion (m/z) | Daughter ion (m/z) |
| Acid Orange II | 40 | 40 | 327.0 | 155.9、79.8 |
5.2 qualitative determination
Each detects target compound and carries out qualitative with (characteristic ion right/quota ion to) pairing LC-MS/MS chromatographic peak area relative abundance of retention time and two pairs of ions.Require the retention time of target compound in the tested sample consistent (consistent condition is that deviation is less than 20%) with the retention time of target compound in the standard solution, require simultaneously two pairs of ion pairs of target compound in the tested sample answer the LC-MS/MS chromatographic peak area than with standard solution in the area of target compound than consistent, relative abundance＞50%, 20-50%, 10-20%,＜10% o'clock, tolerance deviation is respectively 20%, 25%, 30% and 50%.
5.3 quantitative measurement
According to 5.1 liquid chromatography-tandem mass spectrometry condition working samples and matrix mark-on standard solution, to quota ion peak area drawing standard curve, external standard method is quantitative with concentration of standard solution.
6 results calculate
In the formula:
M
1---the sample peak area;
M
2---the base peak area
C---concentration of standard solution, ng/mL
V---constant volume, mL;
M---sample weighting amount, g.
Description of drawings
Accompanying drawing is a typical curve.
Embodiment
Embodiment:
A) take by weighing 1.0 gram samples in the 50mL centrifuge tube, add 10.0mL and extract solution, ultrasonic Extraction 30 minutes, centrifugal 10 minutes of 10000r/min, supernatant are transferred in another 50mL centrifuge tube; Add 10.0mL extraction solution in the residue and extract once more, merge extracted twice solution.
B) purify
Get the 5.0mL sample extracting solution, be settled to 50.0mL with solid-phase extraction column balance solution (2.5) dilution, cross the weak anionic solid-phase extraction column that has activated, with 2mL leacheate, 2mL water wash, 5mL eluent wash-out is collected eluent, blows near with nitrogen and does, be settled to 1.0mL with sample diluting liquid, excessively liquid chromatography tandom mass spectrometry determination behind the 0.22 μ m filter membrane.
C) preparation of matrix mark-on working curve
Take by weighing 1.0 gram blank sample matrix in the 50mL centrifuge tube, take by weighing 6 parts, add standard serial solution (2.15) 100 μ L respectively, operate by 4.1, preparation matrix mark-on working curve, 25,50,100,200,400ng/mL Acid Orange II is:.
D) measure (seeing the typical curve of accompanying drawing):
| Concentration (ng/mL) | 25 | 50 | 100 | 200 | 400 |
| Peak area | 827 | 1980 | 4012 | 7687 | 14730 |
The mensuration of sample precision:
In the sample Acid Orange II content by formula (1) calculate.
Obviously, those of ordinary skill in the art can constitute Acid Orange II Determination on content method with the present invention by the assay method of liquid chromatography-tandem mass spectrometry to Acid Orange II in the food.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (2)
1. illegally added industrial dye-acid orange II Determination on content method in the food is characterized in that described assay method comprises the steps:
Take by weighing sample through centrifugal, ultrasonic Extraction, the utilization solid phase extraction techniques is extracted fluid column and is crossed liquid chromatography tandom mass spectrometry determination behind the 0.22 μ m filter membrane.
2. illegally added industrial dye-acid orange II Determination on content method in a kind of food according to claim 1 is characterized in that: use Solid-Phase Extraction and chromatogram-tandem mass spectrum determination techniques mutually can quantitative measurement food in the content of taurine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100868600A CN101598711A (en) | 2009-06-10 | 2009-06-10 | The assay method of illegally added industrial dye-acid orange II content in a kind of food |
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| CNA2009100868600A CN101598711A (en) | 2009-06-10 | 2009-06-10 | The assay method of illegally added industrial dye-acid orange II content in a kind of food |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915831A (en) * | 2010-08-25 | 2010-12-15 | 南开大学 | Enzyme-linked immunoassay kit for acid orange II |
| CN102608245A (en) * | 2012-03-09 | 2012-07-25 | 天津海世达检测技术有限公司 | Method for rapidly detecting prohibited additive acid orange in red flower by liquid chromatography-mass spectrometry |
| CN103728254A (en) * | 2013-12-20 | 2014-04-16 | 广西中烟工业有限责任公司 | Method for rapidly detecting golden yellow powder in packaging paper |
| CN104807940A (en) * | 2015-05-12 | 2015-07-29 | 广西壮族自治区梧州食品药品检验所 | Method for simultaneously determining multiple illegally-added chemical medicines in health-care food |
| CN104820058A (en) * | 2015-05-12 | 2015-08-05 | 广西壮族自治区梧州食品药品检验所 | Method for determining multiple illegally added chemicals in liquid health food at same time |
| CN104820057A (en) * | 2015-05-12 | 2015-08-05 | 广西壮族自治区梧州食品药品检验所 | Method for determining multiple illegally added chemicals in health food at same time |
| CN110609102A (en) * | 2018-06-14 | 2019-12-24 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for obtaining food extract and application thereof |
-
2009
- 2009-06-10 CN CNA2009100868600A patent/CN101598711A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915831A (en) * | 2010-08-25 | 2010-12-15 | 南开大学 | Enzyme-linked immunoassay kit for acid orange II |
| CN102608245A (en) * | 2012-03-09 | 2012-07-25 | 天津海世达检测技术有限公司 | Method for rapidly detecting prohibited additive acid orange in red flower by liquid chromatography-mass spectrometry |
| CN103728254A (en) * | 2013-12-20 | 2014-04-16 | 广西中烟工业有限责任公司 | Method for rapidly detecting golden yellow powder in packaging paper |
| CN103728254B (en) * | 2013-12-20 | 2016-06-29 | 广西中烟工业有限责任公司 | A kind of method of Acid orange Ⅱ in quick detection wrapping paper |
| CN104807940A (en) * | 2015-05-12 | 2015-07-29 | 广西壮族自治区梧州食品药品检验所 | Method for simultaneously determining multiple illegally-added chemical medicines in health-care food |
| CN104820058A (en) * | 2015-05-12 | 2015-08-05 | 广西壮族自治区梧州食品药品检验所 | Method for determining multiple illegally added chemicals in liquid health food at same time |
| CN104820057A (en) * | 2015-05-12 | 2015-08-05 | 广西壮族自治区梧州食品药品检验所 | Method for determining multiple illegally added chemicals in health food at same time |
| CN110609102A (en) * | 2018-06-14 | 2019-12-24 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for obtaining food extract and application thereof |
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Open date: 20091209 |