CN108387412A - The pre-treating method of detection aquatic products Malachite Green, crystal violet and its metabolite - Google Patents
The pre-treating method of detection aquatic products Malachite Green, crystal violet and its metabolite Download PDFInfo
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- CN108387412A CN108387412A CN201810060294.5A CN201810060294A CN108387412A CN 108387412 A CN108387412 A CN 108387412A CN 201810060294 A CN201810060294 A CN 201810060294A CN 108387412 A CN108387412 A CN 108387412A
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- crystal violet
- malachite green
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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Abstract
The invention discloses a kind of detection aquatic products Malachite Green, the pre-treating methods of crystal violet and its metabolite, belong to the sample pre-treatments in Food Safety Analysis field.The method of the present invention includes measuring samples homogeneous, centrifugation, the activation of solid-phase extraction column, loading, elution.The present invention have many advantages, such as it is simple and easy to do, rapidly and efficiently, accuracy and the rate of recovery it is high, can be used as the common detection methods of aquatic products Malachite Green, concealed malachite green, crystal violet, Recessive Crystal Violet residual quantity.
Description
Technical field
The invention belongs to Food Safety Analysis fields, and in particular to a kind of detection aquatic products Malachite Green, crystal violet and
The pre-treating method of metabolite.
Background technology
Malachite green, crystal violet are a kind of triphenylmethane industrial dyes of synthesis, are applied to textile industry earliest,
Because it is with good anti-bacterial effect, lower-price characteristic, but be widely used in saprolegniasis common in prophylactic treatment fish culture,
Branchiomycosis, ich etc..But Synthesis of diaminodiphenyl has the harm such as high poison, high residue and carcinogenic, teratogenesis, mutagenesis,
And malachite green and crystal violet will produce the stronger leucogentian violet of harmfulness and leuco crystal violet after organism is metabolized.
Therefore, the states such as China and the U.S., Canada, European Union forbid it to be used as the veterinary drug of mankind food fish.However, in numerous water
Still malachite green is being used in the cultivation of product and transportational process.Therefore, in order to ensure food security and meet inlet and outlet
The requirement of detection, establish can Accurate Determining aquatic products Malachite Green, crystal violet and metabolite effective detection method ten
Divide important.
Invention content
The purpose of the present invention is to provide a kind of detection aquatic products Malachite Green, the preceding places of crystal violet and its metabolite
Reason method, have the characteristics that it is simple and easy to do, rapidly and efficiently, filtering after can direct loading, can be used as aquatic products Malachite Green,
The common detection methods of concealed malachite green, crystal violet, Recessive Crystal Violet residual quantity.
In order to achieve this, the present invention adopts the following technical scheme that：
A kind of pre-treating method of detection aquatic products Malachite Green, crystal violet and its metabolite comprising following steps：
（1）Precision weighs 5 g samples in centrifuge tube, 20mL mixed organic solvents is added, then with 10000 rpm/min homogeneous
2 min add 5g alkali aluminas, vibrate 1 min, and then 4500 rpm/min centrifuge 10 min；The mixing is organic molten
Agent is by acetonitrile, formic acid by volume 3:1 mixes；
（2）Take 5 mL steps（1）Gained supernatant adds 5 mL water to dilute, obtains 10mL sample solutions；
（3）C18The activation of neutral alumina solid-phase extraction column：By C18Neutral alumina solid-phase extraction column first uses first containing 2vol%
The acetonitrile solution elution of acid, is then rinsed with the acetonitrile solution of the formic acid containing 20vol% and is cleaned, then after being balanced with distilled water flushing, made
The water surface is preserved higher than cylinder in column；
C18Regeneration method after neutral alumina solid-phase extraction column use is：First rinsed with the acetonitrile solution of the formic acid containing 20vol%
Removal of impurities, then balanced 1 ~ 2 time with distilled water flushing, so that the water surface in column is preserved higher than cylinder；
（4）Sample solution is crossed into column, coutroi velocity is 1 drop/s, is eluted with the aqueous solution of 5 mL acetonitriles containing 20vol% after dripping off, very
Sky is drained, then is eluted with the acetonitrile solution of 2.0 mL formic acid containing 2vol%, is collected eluent in 5 mL scale test tubes, is added 0.1
The ammonium acetate solution of mol/L is settled to 2.5 mL scales；
（5）Vortex mixing, filtering, upper machine examination are tested.
The metabolite includes concealed malachite green, Recessive Crystal Violet.
A kind of detection aquatic products Malachite Green according to the present invention, crystal violet pre-treatment new method distinguishing feature
Sum up as follows：
1）The present invention increases Solid Phase Extraction column technology on the basis of professional standard SN/T 1768-2006 and international standard,
Solid-phase extraction column has a high suction-operated, and can be quickly elute, be remarkably improved the accuracy of detection with it is high
Effect property；
2）The present invention have many advantages, such as it is simple and easy to do, rapidly and efficiently, accuracy and the rate of recovery it is high, can be used as aquatic products Malachite stone
The common detection methods of green, concealed malachite green, crystal violet, Recessive Crystal Violet residual quantity.
Specific implementation mode
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
The preparation of hybrid standard liquid：20.0 mg malachite greens, concealed malachite green, crystal violet and hidden are accurately weighed respectively
Property crystal violet standard items, respectively with acetonitrile dissolve constant volume to 100 mL, obtain hybrid standard storing solution；Accurately pipette appropriate mixing
Standard reserving solution, with dilution in acetonitrile at using standard solution.
Mix the preparation of inner mark solution：1.0 mL malachite greens and concealed malachite green standard solution accurately are pipetted, uses second
Nitrile dilutes constant volume to 50 mL, obtains mixing internal standard storing solution；It is accurate to pipette appropriate mixing internal standard storing solution, with dilution in acetonitrile at
Use inner mark solution.
Embodiment
A kind of pre-treating method of detection sea eel Malachite Green, crystal violet and its metabolite comprising following steps：
（1）Precision weighs 5 g samples in centrifuge tube, 20mL mixed organic solvents is added, then with 10000 rpm/min homogeneous
2 min add 5g alkali aluminas, vibrate 1 min, and then 4500 rpm/min centrifuge 10 min；The mixing is organic molten
Agent is by acetonitrile, formic acid by volume 3:1 mixes；
（2）Take 5 mL steps（1）Gained supernatant adds 5 mL water to dilute, obtains 10mL sample solutions（If sample solution muddiness can be with
10000 rpm/min centrifuge 3 min again）；
（3）C18The activation of neutral alumina solid-phase extraction column：By C18Neutral alumina solid-phase extraction column is first contained with 2 mL
The acetonitrile solution of 2vol% formic acid elutes, and is then rinsed and is cleaned with the acetonitrile solution of 5 mL formic acid containing 20vol%, then distilled with 3 mL
After water rinses balance, remaining 1 mL water closes valve, it is spare that one 30 mL dilatation pipes is filled on column in column；
（4）Sample solution is crossed into column, coutroi velocity is 1 drop/s, is eluted with the aqueous solution of 5 mL acetonitriles containing 20vol% after dripping off, very
Sky is drained, then is eluted with the acetonitrile solution of 2.0 mL formic acid containing 2vol%, is collected eluent in 5 mL scale test tubes, is added 0.1
The ammonium acetate solution of mol/L is settled to 2.5 mL scales；
（5）Vortex mixing, filtering, upper machine examination are tested.
Detection limit of the present invention to blank sea eel sample Malachite Green, concealed malachite green, crystal violet, Recessive Crystal Violet
For 0.1 μ g/kg, meet national standard.
The recycling of sea eel Malachite Green, crystal violet, concealed malachite green, Recessive Crystal Violet is detected using the method for the present invention
Rate is as a result as follows：
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with repair
Decorations should all belong to the covering scope of the present invention.
Claims (3)
1. the pre-treating method of a kind of detection aquatic products Malachite Green, crystal violet and its metabolite, it is characterised in that：Including
Following steps：
（1）Precision weighs 5 g samples in centrifuge tube, 20mL mixed organic solvents is added, then with 10000 rpm/min homogeneous
2 min add 5g alkali aluminas, vibrate 1 min, and then 4500 rpm/min centrifuge 10 min；
（2）Take 5 mL steps（1）Gained supernatant adds 5 mL water to dilute, obtains 10mL sample solutions；
（3）C18The activation of neutral alumina solid-phase extraction column：By C18Neutral alumina solid-phase extraction column first uses formic acid containing 2vol%
Acetonitrile solution elution, then rinsed and cleaned with the acetonitrile solution of the formic acid containing 20vol%, then after being balanced with distilled water flushing, make column
The middle water surface is preserved higher than cylinder；
（4）Sample solution is crossed into column, coutroi velocity is 1 drop/s, is eluted with the aqueous solution of 5 mL acetonitriles containing 20vol% after dripping off, very
Sky is drained, then is eluted with the acetonitrile solution of 2.0 mL formic acid containing 2vol%, is collected eluent in 5 mL scale test tubes, is added 0.1
The ammonium acetate solution of mol/L is settled to 2.5 mL scales；
（5）Vortex mixing, filtering, upper machine examination are tested.
2. the pre-treating method of detection aquatic products Malachite Green according to claim 1, crystal violet and its metabolite,
It is characterized in that：The metabolite includes concealed malachite green, Recessive Crystal Violet.
3. the pre-treating method of detection aquatic products Malachite Green according to claim 1, crystal violet and its metabolite,
It is characterized in that：Step（1）Described in mixed organic solvents be by acetonitrile and formic acid by volume 3:1 cooperation is made.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810060294.5A CN108387412A (en) | 2018-01-22 | 2018-01-22 | The pre-treating method of detection aquatic products Malachite Green, crystal violet and its metabolite |
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| CN201810060294.5A CN108387412A (en) | 2018-01-22 | 2018-01-22 | The pre-treating method of detection aquatic products Malachite Green, crystal violet and its metabolite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109655549A (en) * | 2019-01-24 | 2019-04-19 | 梧州市食品药品检验所 | A kind of method of quick detection fish Malachite Green |
| CN110333215A (en) * | 2018-12-29 | 2019-10-15 | 厦门市普识纳米科技有限公司 | A kind of detection method of aquatic products Malachite Green and crystal violet |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2039425U (en) * | 1988-09-08 | 1989-06-14 | 河北省津杨滤材厂 | Chromatographic preprocessing column |
| CN102980961A (en) * | 2012-12-19 | 2013-03-20 | 福州大学 | Pretreatment method of detection on malachite green, crystal violet and residues of malachite green and crystal violet in eels |
| CN104730157A (en) * | 2013-12-23 | 2015-06-24 | 天津优标技术检测服务有限公司 | Method for detecting residues of malachite green in health products by using UPLC-MS |
| WO2016100383A1 (en) * | 2014-12-15 | 2016-06-23 | BugCo, Inc. | Compositions and methods for detecting pathogens |
| CN106731181A (en) * | 2016-12-05 | 2017-05-31 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of decontaminating column of extract solution direct injected |
-
2018
- 2018-01-22 CN CN201810060294.5A patent/CN108387412A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2039425U (en) * | 1988-09-08 | 1989-06-14 | 河北省津杨滤材厂 | Chromatographic preprocessing column |
| CN102980961A (en) * | 2012-12-19 | 2013-03-20 | 福州大学 | Pretreatment method of detection on malachite green, crystal violet and residues of malachite green and crystal violet in eels |
| CN104730157A (en) * | 2013-12-23 | 2015-06-24 | 天津优标技术检测服务有限公司 | Method for detecting residues of malachite green in health products by using UPLC-MS |
| WO2016100383A1 (en) * | 2014-12-15 | 2016-06-23 | BugCo, Inc. | Compositions and methods for detecting pathogens |
| CN106731181A (en) * | 2016-12-05 | 2017-05-31 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of decontaminating column of extract solution direct injected |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局 等: "《水产品中孔雀石绿和结晶紫残留量的测定 GB/T 19857-2005》", 5 September 2005 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110333215A (en) * | 2018-12-29 | 2019-10-15 | 厦门市普识纳米科技有限公司 | A kind of detection method of aquatic products Malachite Green and crystal violet |
| CN109655549A (en) * | 2019-01-24 | 2019-04-19 | 梧州市食品药品检验所 | A kind of method of quick detection fish Malachite Green |
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Application publication date: 20180810 |