CN103105367A - Method for rapidly detecting malachite green or crystal violet in aquaculture water - Google Patents
Method for rapidly detecting malachite green or crystal violet in aquaculture water Download PDFInfo
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- CN103105367A CN103105367A CN2013100263375A CN201310026337A CN103105367A CN 103105367 A CN103105367 A CN 103105367A CN 2013100263375 A CN2013100263375 A CN 2013100263375A CN 201310026337 A CN201310026337 A CN 201310026337A CN 103105367 A CN103105367 A CN 103105367A
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- malachite green
- crystal violet
- aquaculture water
- sample solution
- fast detecting
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- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 title claims abstract description 51
- 229940107698 malachite green Drugs 0.000 title claims abstract description 49
- 239000013078 crystal Substances 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000009360 aquaculture Methods 0.000 title claims abstract description 24
- 244000144974 aquaculture Species 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000012074 organic phase Substances 0.000 claims abstract description 3
- 239000012488 sample solution Substances 0.000 claims description 12
- 239000012086 standard solution Substances 0.000 claims description 12
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004439 Isononyl alcohol Substances 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 150000003333 secondary alcohols Chemical class 0.000 claims description 3
- QDTDKYHPHANITQ-UHFFFAOYSA-N 7-methyloctan-1-ol Chemical compound CC(C)CCCCCCO QDTDKYHPHANITQ-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- -1 polyethylene octyl phenyl ether Polymers 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 12
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000000638 solvent extraction Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 9
- 241000252233 Cyprinus carpio Species 0.000 description 7
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 241000238557 Decapoda Species 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- ZXJXZNDDNMQXFV-UHFFFAOYSA-M crystal violet Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1[C+](C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 ZXJXZNDDNMQXFV-UHFFFAOYSA-M 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 208000037088 Chromosome Breakage Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000002141 anti-parasite Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000005886 chromosome breakage Effects 0.000 description 1
- 238000000136 cloud-point extraction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 208000010824 fish disease Diseases 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000004885 tandem mass spectrometry Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 239000000273 veterinary drug Substances 0.000 description 1
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- Farming Of Fish And Shellfish (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for rapidly detecting malachite green or crystal violet in aquaculture water, which comprises the steps of using a rapid synergic solvent extraction system formed by auxiliary extraction agent, extraction agent and water to extract the crystal violet or the malachite green into organic phase at the upper part of a centrifuge tube; and detecting the malachite green or the crystal violet in the sample by comparing the standard content of the malachite green or the crystal violet, wherein the limit of detection is 0.05mu g/mL. Compared with the existing detection methods, the method is mild in extraction conditions and rapid in detection; the whole analysis and detection process can be completed within 5-10min; and the method is low in cost, does not need a large instrument and is high in accuracy, thus being suitable for detecting the safety of edible aquatic products and having great utilization potentiality and wide market prospect.
Description
Technical field
The present invention relates to malachite green in a kind of fast detecting aquaculture water or the method for crystal violet, belong to food animal forbidding adjuvant detection technique.
Background technology
Malachite green and crystal violet all belong to triphenylmethane dye, and its lovely luster is with low cost, is widely used in aquaculture, food, medical treatment and textile industry.Along with the development of science and technology, people find that gradually these two kinds of compounds are to the harm of human body.Because malachite green and crystal violet have sterilization and anti parasitic effect, can prevent and treat various fish diseases, be widely used in culture fishery.But it is carcinogenic that itself and metabolic product all have, teratogenesis, and mutagenesis makes the effects such as chromosome breakage and respiratory system toxicity.Malachite green and crystal violet are forbidden in culture fishery by European Union and U.S. FDA.For fear of edible animal, the healthy of consumer worked the mischief, 2002, also classify malachite green as forbidden drugs in No. 193 bulletin of China Ministry of Agriculture " veterinary drug and other compound inventory of food animal forbidding ".But, due to its good anti-bacterial effect, low price, many raisers are still at Misuse, and therefore, the residual monitoring of malachite green and crystal violet just seems especially important.
The method that detects at present malachite green and crystal violet mainly contains: high performance liquid chromatography (HPLC), liquid chromatography-mass spectrography (HPLC-MS), Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS-MS), Internal standard.These methods need to be used the large-scale instruments such as HPLC, MS, and cost is high, and length consuming time is not suitable for Site Detection.
The fast synergistic abstraction technique is a kind of novel eco-friendly solute enrichment and separation method, yet there are no and utilize the fast synergistic extraction malachite green and crystal violet to be carried out the report of extract and separate, what reported is that cloud point extraction is to the extracting and enriching of malachite green and crystal violet, need heating, need analysis time dozens of minutes just can complete.The characteristics such as the present invention has adopted surfactant to help malachite green and crystal violet in extraction agent-extractant-water fast synergistic extraction aquaculture water, has normal-temperature operation, detects that quick 5-10min can complete detection, result is accurate, and is highly sensitive, and cost is low.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method of fast detecting aquaculture water Malachite Green or crystal violet is provided, when guaranteeing accuracy in detection and sensitivity, reduce testing cost, shorten detection time.
Purpose of the present invention is achieved by the following technical programs:
(1) get that 5mL contains the sample solution of malachite green or crystal violet and the standard solution of 5mL malachite green or crystal violet is placed in 10mL tool plug centrifuge tube, add respectively in standard solution and sample solution and help extraction agent surfactant and extractant, vortex, centrifugal;
(2) color of more centrifugal rear both upper organic phase, if the color of sample solution is deeper than standard solution, interpret sample solution Malachite Green or crystal violet content is greater than the content of the malachite green in standard solution or crystal violet, on the contrary interpret sample solution Malachite Green or crystal violet content less than the content in standard solution.
Described in step in the present invention (1) contain malachite green or the crystal violet sample solution refers to aquaculture water, malachite green or crystal violet concentration of standard solution are 0.05-0.2 μ g/mL.
In the present invention, extractant is a kind of in octanol, isooctyl alcohol, an alcohol, isononyl alcohol, and consumption is 0.2-0.5mL.
It is a kind of in surfactant polyethylene octyl phenyl ether (Triton-100 or Triton-114), NPE (Np-7 or Np-9), branched secondary alcohol polyoxyethylene ether (TMN-6) helping the extraction agent in the present invention, helping extraction agent concentration of volume percent is 5%-10% (v/v), and consumption is 10-50 μ l.
Mesoscale eddies time 5-30s of the present invention, centrifugation time 3-8min, centrifugation rate 2500-5000r/min.
With respect to prior art, the present invention has following remarkable advantage:
1, utilization of the present invention helps extraction agent-extractant-water fast synergistic extraction as the pre-treating method of example enrichment, malachite green or crystal violet are enriched in the very little extractant of volume, enrichment times reaches 50 times, before enrichment, solution is colourless, after enrichment, blue-green or purple ring appear in the centrifuge tube upper strata, color is obvious, is easy to observe, and detectability can reach 0.05 μ g/mL;
2, need not to purchase the expensive checkout equipments such as HPLC, MS, test required instrument simple, mild condition, easy and simple to handle, accuracy is high, and the layman also can complete, 5-10min can complete whole analyte detection process, for quality testing department provides a kind of quick, easy, directly perceived, economic detection aquaculture water Malachite Green or the method for crystal violet, be applicable to the detection of edible aquatic products safety, this method has very large application potential and wide market application foreground.
Embodiment
Below in conjunction with embodiment, the present invention is further described, but protection scope of the present invention is not limited to this.
Embodiment 1:The method of the malachite green in fast detecting aquaculture water, concrete operations are as follows:
1. 5mL eel culture water and concentration are respectively 0.05,0.1,0.15,0.2 each 5mL of malachite green standard serial solution of μ g/mL is placed in 10ml tool plug centrifuge tube, adding 300 μ l isooctyl alcohol and 10 μ l Triton X-100 Triton-100(concentration of volume percent in every centrifuge tube is 10%); Vortex 5s forms uniform opaque system; Centrifugal 3 min under 3500 r/min conditions, breakdown of emulsion, phase-splitting, extractant is at centrifuge tube top formation one deck ring, and malachite green is extracted in this one deck ring; 2. under the same terms, eel culture water is compared at the bluish-green colour circle of one deck of centrifuge tube top formation and one deck colour circle color range of standard serial solution formation, the color of the colour circle that eel culture water forms is darker than the color that 0.2 μ g/mL standard malachite green forms, and eel culture water Malachite Green content is higher than 0.2 μ g/mL.
Embodiment 2:The method of the crystal violet in fast detecting aquaculture water, concrete operations are as follows:
1. 5mL carp culture water and concentration are respectively 0.05,0.1,0.15 each 5mL of crystal violet standard serial solution of μ g/mL is placed in 10ml tool plug centrifuge tube, add 200 μ l octanols and 50 μ l NPE Np-7 (concentration of volume percent is 5%) in every centrifuge tube, vortex 20s forms uniform opaque system; Centrifugal 5min under 4000 r/min conditions, breakdown of emulsion, phase-splitting, extractant is at centrifuge tube top formation one deck ring, and crystal violet is extracted in this one deck ring; 2. under the same terms, carp culture water is compared at one deck purple ring of centrifuge tube top formation and the colour circle of standard serial solution formation, the color of the colour circle that carp culture water forms is more of light color than 0.05 μ g/mL standard knots crystalviolet formation, and in carp culture water, crystal violet content is lower than 0.05 μ g/mL.
Embodiment 3:The method of the malachite green in fast detecting aquaculture water, concrete operations are as follows:
1. 5mL shrimp aquaculture water and concentration are respectively 0.05,0.1,0.15 each 5mL of malachite green standard serial solution of 0.2 μ g/mL is placed in tool plug centrifuge tube, adding 500 μ l to appoint pure and mild 20 μ l branched secondary alcohol polyoxyethylene ether TMN-6(concentration of volume percent in every centrifuge tube is 10%); Vortex 15s forms uniform opaque system; Centrifugal 6min under 2500 r/min conditions, breakdown of emulsion, phase-splitting, extractant is at centrifuge tube top formation one deck ring, and malachite green is extracted in this one deck ring; 2. under the same terms, shrimp aquaculture water is compared at the bluish-green colour circle of one deck of centrifuge tube top formation and one deck colour circle color range of standard serial solution formation, the color of the ring that shrimp aquaculture water forms is between between the colour circle that 0.05-0.1 μ g/mL standard malachite green forms, and the content of shrimp aquaculture water Malachite Green is between between 0.05-0.1 μ g/mL.
Above embodiment and high performance liquid chromatography comparative result see Table 1.
Table 1: embodiment result and high performance liquid chromatography comparative result
By table 1 result as can be known: the content of the aquaculture water Malachite Green of measuring with the present invention is more identical with the content results of the malachite green of the high effective liquid chromatography for measuring of national standard employing, and illustration method has certain reliability.The method fast and easy of this invention malachite green that detects, result is accurately that other method is very inaccessible.
Embodiment 4:The method of the crystal violet in fast detecting aquaculture water, concrete operations are as follows:
1. 5mL crucian cultivation water and concentration are respectively 0.05,0.1,0.15,0.2 each 5mL of crystal violet standard serial solution of μ g/mL is placed in 10ml tool plug centrifuge tube, add 400 μ l isononyl alcohols and 30 μ l NPE Np-9 (concentration of volume percent is 8%) in every centrifuge tube, vortex 30s forms uniform opaque system; Centrifugal 8min under 5000 r/min conditions, breakdown of emulsion, phase-splitting, extractant is at centrifuge tube top formation one deck ring, and crystal violet is extracted in this one deck ring; 2. under the same terms, carp culture water is compared at one deck purple ring of centrifuge tube top formation and the colour circle of standard serial solution formation, the color of the colour circle that carp culture water forms is between between the color that 0.1-0.15 μ g/mL standard knots crystalviolet forms, and in carp culture water, crystal violet content is between between 0.1-0.15 μ g/mL.
Claims (5)
1. the method for a fast detecting aquaculture water Malachite Green or crystal violet comprises the following steps:
(1) get that 5mL contains the sample solution of malachite green or crystal violet and the standard solution of 5mL malachite green or crystal violet is placed in tool plug centrifuge tube, add respectively in standard solution and sample solution and help extraction agent and extractant, vortex, centrifugal;
(2) color of more centrifugal rear both upper organic phase, if the color of sample solution is deeper than standard solution, interpret sample solution Malachite Green or crystal violet content is greater than the content of the malachite green in standard solution or crystal violet, on the contrary interpret sample solution Malachite Green or crystal violet content less than the content in standard solution.
2. the method for fast detecting aquaculture water Malachite Green according to claim 1 or crystal violet, it is characterized in that: described in step (1) contain malachite green or the crystal violet sample solution is aquaculture water, malachite green or crystal violet concentration of standard solution are 0.05-0.2 μ g/mL.
3. the malachite green in fast detecting aquaculture water according to claim 1 or the method for crystal violet is characterized in that: extractant is octanol, isooctyl alcohol, appoint a kind of in alcohol, isononyl alcohol, and consumption is 0.2-0.5mL.
4. the malachite green in fast detecting aquaculture water according to claim 1 or the method for crystal violet, it is characterized in that: helping the extraction agent is a kind of in surfactant polyethylene octyl phenyl ether Triton-100, Triton X-100 Triton-114, NPE Np-7, NPE Np-9, branched secondary alcohol polyoxyethylene ether TMN-6, helping extraction agent concentration of volume percent is 5-10%, and consumption is 10-50 μ l.
5. the malachite green in fast detecting aquaculture water or the method for crystal violet according to claim 1, it is characterized in that: vortex time is 5-30s, and centrifugation time is 3-8min, and centrifugation rate is 2500-5000r/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103583436A (en) * | 2013-11-13 | 2014-02-19 | 叶大铿 | Detoxification, fishy smell elimination and freshness increase farming method for Egypt clarias fuscus |
| CN109633032A (en) * | 2019-01-25 | 2019-04-16 | 云南省农业科学院农产品加工研究所 | Method that is a kind of while measuring malachite green and crystal violet content |
| CN109932352A (en) * | 2019-03-15 | 2019-06-25 | 上海如海光电科技有限公司 | A kind of Raman detection method of aquatic products Malachite Green and crystal violet |
| CN111380852A (en) * | 2018-12-28 | 2020-07-07 | 普拉瑞思科学仪器（苏州）有限公司 | Surface-enhanced Raman spectroscopy rapid detection method for malachite green, crystal violet and recessive substances thereof in aquatic products |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103583436A (en) * | 2013-11-13 | 2014-02-19 | 叶大铿 | Detoxification, fishy smell elimination and freshness increase farming method for Egypt clarias fuscus |
| CN103583436B (en) * | 2013-11-13 | 2015-04-22 | 广州市正源生态农业有限公司 | Detoxification, fishy smell elimination and freshness increase farming method for Egypt clarias fuscus |
| CN111380852A (en) * | 2018-12-28 | 2020-07-07 | 普拉瑞思科学仪器（苏州）有限公司 | Surface-enhanced Raman spectroscopy rapid detection method for malachite green, crystal violet and recessive substances thereof in aquatic products |
| CN109633032A (en) * | 2019-01-25 | 2019-04-16 | 云南省农业科学院农产品加工研究所 | Method that is a kind of while measuring malachite green and crystal violet content |
| CN109633032B (en) * | 2019-01-25 | 2022-04-05 | 云南省农业科学院农产品加工研究所 | Method for simultaneously measuring content of malachite green and crystal violet |
| CN109932352A (en) * | 2019-03-15 | 2019-06-25 | 上海如海光电科技有限公司 | A kind of Raman detection method of aquatic products Malachite Green and crystal violet |
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