CN106093242B - The rapid detection method of sulfa drug residue in one seed shrimp - Google Patents
The rapid detection method of sulfa drug residue in one seed shrimp Download PDFInfo
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Abstract
The invention discloses the rapid detection methods of sulfa drug residue in a seed shrimp, sulfa drug residue in shrimp is extracted using methanol, pass through sulfa drug residue and the quick derivatization reaction of specific derivatization reagent, form stable aubergine derivative, colour developing result is visually observed from realization quickly detection, the minimum reachable 50 μ g/kg of detection sensitivity.Pre-treatment of the present invention is simple, and detection time is short, and testing cost is low, is not necessarily to large-scale instrument, can Site Detection, visual color variation can quickly obtain testing result, can quickly, sulfa drug residue in efficient detection shrimp.
Description
Technical field
The present invention relates to a kind of detection method of sulfa drug residue in aquatic products, more particularly to sulfamido in a seed shrimp
The rapid detection method of medicament residue.
Background technology
Sulfa drugs is the general name of the synthetic antibiotic based on P-aminobenzene-sulfonamide structure, is a kind of be used in advance
Anti- and treatment bacterial infection disease chemotherapeutic agent.In recent years, with both at home and abroad to the analysis of sulfa drug residue
Many-sided research has been carried out, the method for many detection sulfa drugs, including high performance liquid chromatography has occurred（Such as
CN101639466A）, liquid chromatography-mass spectrometry, colloidal gold immunity chromatography, immunoassay and near infrared spectroscopy etc..But
Only pay attention to laboratory traditional detection, and there are sample pre-treatments step complexity, consuming time length, small throughput, limits of high cost
System.However, the Fast Detection Technique of aquatic products drug residue is very deficient, the traditional detection mode in current experiment room is difficult reality
Now fast and efficiently detection result, is increasingly not suitable with the production, circulation and sales feature of food.
Invention content
The purpose of the present invention is to provide the rapid detection methods of sulfa drug residue in a seed shrimp, and pre-treatment is simple,
Detection time is short, and testing cost is low, be not necessarily to large-scale instrument, can Site Detection, visual color variation can quickly be examined
Survey as a result, it is possible to quickly, sulfa drug residue in efficient detection shrimp.
The technical solution adopted by the present invention to solve the technical problems is：
The rapid detection method of sulfa drug residue, includes the following steps in one seed shrimp：
（1）Sample pre-treatments：Shrimp grinding is homogenized to obtain shrimp slurry, takes shrimp to starch 5.0g, add by the shrimp for taking fresh prawns
Enter the anhydrous sodium sulfate and methanol 20mL of 5.0g, after shaking 2 minutes, stratification or 4000 turns/min centrifuge 5min, on gained
Clear liquid is as sample treatment liquid；
（2）Detection：2mL derivatization reagents 01 are added in 5mL sample treatment liquids, shaking is added 0.1mL and derives after five minutes
Change reagent 02, shaking 1 minute stands 5 minutes, the supernatant liquid color after observation is derivative, shows if the aobvious red of supernatant liquid
Contain sulfa drugs in sample, content is more than 100 μ g/kg；If the not aobvious red of supernatant liquid, is handled using chromatographic column
Secondary detection afterwards.
Inventor develops the specific rapid detection method of sulfa drug residue in suitable shrimp by studying for a long period of time.This
The principle of invention：Using column front derivation, chemical staining method.The present invention extracts the sulfa drug residue in shrimp using methanol,
By sulfa drug residue and the quick derivatization reaction of specific derivatization reagent, stable aubergine derivative is formed, naked eyes
Observation colour developing result is quickly detected from realization, the minimum reachable 50 μ g/kg of detection sensitivity.This method detection limit meet European Union and I
Demand of the state to sulfonamides analyte detection, and can realize the field quick detection of a variety of sulfa drugs in shrimp.
Anhydrous sodium sulfate and methanol is added in the present invention simultaneously in shrimp slurry, and methanol is used to extract the sulfonamides in shrimp
Object remains, and anhydrous sodium sulfate can exclude the interference of moisture, meanwhile, anhydrous sodium sulfate can make shrimp tissue dispersion evenly,
Conducive to methanol more rapidly, efficiently extract sulfa drug residue.
After the derivatization reagent that sample treatment liquid is selected through the present invention derives, sulfa drugs content is more than 100 μ g/kg
Sample can see apparent chromogenic reaction, so as to quickly obtain testing result.And in order to further increase the essence of detection
Degree, to sample of the sulfa drugs content under 100 μ g/kg, the derivatization reagent that sample treatment liquid is selected through the present invention spreads out
After life, does not develop the color substantially or naked eyes are difficult to observe by colour developing, the present invention is handled using specific chromatographic column to upper after derivative
Layer liquid concentration observes colour developing as a result, for sulfa drugs content more than 50 μ g/kg, under 100 μ g/kg again after elution
Sample, it can be seen that apparent chromogenic reaction, further improve the present invention accuracy of detection, meet higher detection demand.
Scheme as an optimization, the rapid detection method of sulfa drug residue, includes the following steps in a seed shrimp：
（1）Sample pre-treatments：Shrimp grinding is homogenized to obtain shrimp slurry, takes shrimp to starch 5.0g, add by the shrimp for taking fresh prawns
Enter the anhydrous sodium sulfate and methanol 20mL of 5.0g, after shaking 2 minutes, stratification or 4000 turns/min centrifuge 5min, on gained
Clear liquid is as sample treatment liquid；
（2）Detection：2mL derivatization reagents 01 are added in 5mL sample treatment liquids, shaking is added 0.1mL and derives after five minutes
Change reagent 02, shake 1 minute, stands and detected after directly using chromatographic column processing after five minutes.Operation is detected after chromatographic column processing
For：A, chromatographic column activates：2mL methanol and 5mL distilled water are sequentially added in chromatographic column, coutroi velocity is 1-2 drops/sec, is discarded
Efflux；B, chromatography detection：Supernatant liquid is added in the chromatographic column after A step activation, 2mL deionized waters elution column is added
Son is drained；Finally plus 0.8mL ethyl acetate elutes, and wash water color is observed, if eluent displaing amaranth, shows in sample
Containing sulfanilamide (SN) substance, content is more than 50 μ g/kg.
Preferably, secondary detection operation is after chromatographic column processing：
A, chromatographic column activates：2mL methanol and 5mL distilled water are sequentially added in chromatographic column, coutroi velocity is 1-2 drops/sec,
Discard efflux；
B, chromatography detection：Supernatant liquid is added in the chromatographic column after A step activation, 2mL deionized waters elution column is added
Son is drained；Finally plus the elution of 0.8mL ethyl acetate, observation wash water color show to contain in sample if eluent is aobvious red
There is sulfanilamide (SN) substance, content is more than 50 μ g/kg, under 100 μ g/kg.
Preferably, step（2）The aobvious red specially supernatant liquid displaing amaranth of liquid at the middle and upper levels.
Preferably, the aobvious red specially eluent displaing amaranth of eluent in step B.
Preferably, loading the mixture of HLB reverse-phase chromatographies filler and silica filler, HLB reverse phase colors in the chromatographic column
The mass ratio for composing filler and silica filler is 4：1.The filler of chromatographic column filling of the present invention has particular requirement, to be suitble to after deriving
Supernatant liquid can just play the role of apparent concentration, improve detection result.HLB reverse-phase chromatographies filler has derivative very strong
Extraction concentration derivative ability, silica filler not only has the ability that very strong extraction concentrates derivative, and can also press down
The adsorption capacity of protein, reduces the interference of protein in shrimp sample processed.The two is used in combination, and obtains good inspissation.
Preferably, the HLB reverse-phase chromatographies filler average particle size：40-60 μm, average pore size：80Å.
Preferably, the silica filler average particle size：40-60 μm, average pore size：50Å.
Preferably, step（2）Regulation system pH value is 12 after middle addition 2mL derivatization reagents 01.
Preferably, 01 specific ingredient of the derivatization reagent is the sodium carbonate liquor of mass concentration 5%.
Preferably, the derivatization reagent 02 specifically comprises：The nitrous acid solution of mass concentration 5%, mass concentration 5%
Aqueous solution of urea and mass concentration 0.1% beta naphthal ethanol solution according to 1:1:The mixture of 2 volume ratio.
The beneficial effects of the invention are as follows：Pre-treatment is simple, and detection time is short, and testing cost is low, is not necessarily to large-scale instrument, can show
Field detecting, visual color variation can quickly obtain testing result, can quickly, in efficient detection shrimp sulfa drugs is residual
It stays.
Specific implementation mode
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art.
Method in following embodiments is unless otherwise instructed the conventional method of this field.
Sulfa drugs standard items（It is commercially available）：Sulphadiazine, sulfamethyldiazine, sulfamonomethoxine, methylene sulfonamide
Isoxazole；Sample is fresh prawns, is purchased from Zhoushan Aquatic Wholesale Market.
Derivatization reagent 01, derivatization reagent 02 are commercially available, are purchased from the product of Beijing Liujiaoti Science ＆ Technology Development Co., Ltd.
" tissue sample sulfamido quick detection kit ", derivatization reagent 01 are the reagent A in kit, and derivatization reagent 02 is
Reagent B, reagent C, reagent D in kit is according to 1:1:2 volume ratio mixes.
It is furthermore preferred that derivatization reagent 01, derivatization reagent 02 oneself can also be prepared：The derivatization reagent 01 specifically at
It is divided into the sodium carbonate liquor of mass concentration 5%, the derivatization reagent 02 specifically comprises：The nitrous acid solution of mass concentration 5%,
The aqueous solution of urea of mass concentration 5% is with the beta naphthal ethanol solution of mass concentration 0.1% according to 1:1:The mixing of 2 volume ratio
Object.
Embodiment：
1, the detection of sulfa drugs standard substance
Sulfa drugs standard items are dissolved to methanol and are diluted to the concentration of 50 μ g/L, 100 μ g/L.Take 1mL dense respectively
Degree is 50 μ g/L, 100 μ g/L sulfa drugs standard solution, and the methanol and 2mL derivatization reagents 01 of 4mL is added, and shakes 5 points
0.1mL derivatization reagents 02 are added after clock, shake 1 minute, stand 5 minutes, observe supernatant liquid color；5 repetitions each are done,
Do reagent blank experiment simultaneously.
2, sample detection
2.1 take the shrimp of fresh prawns, and shrimp grinding is homogenized to obtain shrimp slurry, takes shrimp to starch 5.0g, the nothing of 5.0g is added
Aqueous sodium persulfate and methanol 20mL, after shaking 2 minutes, stratification or 4000 turns/min centrifuge 5min, and gained supernatant is as sample
Product treatment fluid.
2.2 are added 2mL derivatization reagents 01 in 5mL sample treatment liquids, and adjust pH=12, and shaking is added after five minutes
0.1mL derivatization reagents 02 shake 1 minute, stand 5 minutes, observe supernatant liquid color；It is preliminary to judge：In 5mL sample treatments
2mL derivatization reagents 01 are added in liquid, 0.1mL derivatization reagents 02 are added in shaking after five minutes, shake 1 minute, stand 5 minutes,
Supernatant liquid color after observation is derivative, shows to contain sulfa drugs, content in sample if supernatant liquid displaing amaranth
More than 100 μ g/kg；If supernatant liquid not displaing amaranth or colour developing unobvious（Naked eyes are difficult to distinguish）, then use at chromatographic column
Secondary detection after reason.
Secondary detection, which operates, after chromatographic column processing is：Chromatographic column one is taken to sequentially add 2mL methanol and 5mL distilled water in layer
It analyses in column, coutroi velocity is 1-2 drops/sec, discards efflux；Supernatant liquid after derivative is added in the chromatographic column after activation, then
2mL deionized waters are added and elute pillar, drain；Finally plus 0.8mL ethyl acetate elutes, and observes wash water color；As a result judge：
Eluent observes color when volatilizing naturally：If displaing amaranth, show to contain sulfanilamide (SN) substance in sample, content is in 50 μ
G/kg or more, do not develop the color or develop the color unobvious（Naked eyes are difficult to distinguish）Then show to be less than 50 containing sulfamido content of material in sample
μ g/kg, to more accurate detection, it is necessary to further be detected with large-scale instrument such as high performance liquid chromatography etc..
HLB reverse-phase chromatography fillers are loaded in chromatographic column（It is commercially available, average particle size：40-60 μm, average pore size：80Å）And silica gel
Filler（It is commercially available, HisepTMSilica filler, average particle size：40-60 μm, average pore size：50Å）Mixture, HLB reverse-phase chromatographies fill out
The mass ratio of material and silica filler is 4：1,
3, the condition optimizing of sample pre-treatments
Influence of 3.1 pH value to derivatization effect
100 μ g/kg sulfa drugs standard solution 1mL are taken, the methanol of 4 mL is added, adds derivatization reagent 01（It adjusts
It is respectively 6,8,10,12 to save pH value）, it is performed the derivatization according to Section 1 step, directly observes the derivatization effect under different pH value,
To select best derivatization pH value.The result shows that when pH value is 6, no color change；When pH value >=8, color changes,
And alkalinity is bigger, color is redder, therefore when pH value is 12, and derivative effect is ideal.
3.2 chromatographic columns it is preferred
By supernatant liquid of second section after derivative, chromatographic column, silicagel column respectively through the present invention（It is commercially available）, HLB columns（City
It sells）, alumina column（It is commercially available）, ENVI-18 solid phase extraction columns（It is commercially available）Concentration and purification, the processing side provided according to each column
The color change of eluent is observed in method, successively activation, balance, loading, elution and elution respectively.The result shows that chromatographic column, silicon
Rubber column gel column, HLB columns, alumina column, ENVI-18 with a hook at the end, but the chromatographic column reservation efficiency of the present invention is best.
The detection of sulfa drug residue in shrimp sample
Sulfa drugs standard substance derivative is in apparent aubergine, and with the increase color burn of content, blank
Control then not aobvious discoloration.As a concentration of 50 μ g/L or more of sulfa drugs standard substance, derivative is in centrifuge tube in purple
It is red.The derivative is subjected to chromatographic column concentration and purification, the color in chromatographic column become apparent from, the color after elution is placed
200min is without significant change.
Add Precision Experiment result
Sulfa drugs standard is carried out to the blank sample of 60 parts of known contents and adds verification test, standard substance addition contains
Amount is respectively 50 μ g/kg, 100 μ g/kg, and confirmatory experiment is carried out according to Section 1 method by different operation personnel.Work as sulfa drugs
Residual addition concentration is when being respectively 50 μ g/kg, 100 μ g/kg, can be observed apparent purplish red colour developing, and negative sample is without going out
Existing color change.
Comparison experimental result
According to GB/T 21316-2007 methods 325 parts are detected using the method for Liquid Chromatography-Tandem Mass Spectrometry instrument and the present invention
Sulfa drug residue in the blind sample of prawn, the two result are compared.Liquid chromatography tandem mass spectrometry is detected containing sulfanilamide (SN)
The sample of class medicament residue has 62, and total content range is higher than the sample of 50 μ g/kg in 2.0 μ g/kg-103.5 μ g/kg, total content
Product have 16.The method of the present invention quickly detects 325 parts of samples, and sulfa drug residue content is in 50.0 μ g/kg -103.5 μ
16 samples between g/kg have different degrees of chromogenic reaction, the two result to meet.
Conclusion
Shrimp samples of the present invention are extracted using methanol, and chromatographic column purification enrichment performs the derivatization reaction under alkaline condition,
Derivatization product keeps relative stability in 200min, and detection is completed in 30min, realizes the quick of sulfa drug residue
Screening, method quickly, it is accurate, practical, can sulfa drug residue in Effective selection shrimp.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, on the premise of not exceeding the technical scheme recorded in the claims also other variations and modifications.
Claims (9)
1. the rapid detection method of sulfa drug residue in a seed shrimp, which is characterized in that include the following steps：
（1）Sample pre-treatments：Shrimp grinding is homogenized to obtain shrimp slurry, takes shrimp to starch 5.0g, be added by the shrimp for taking fresh prawns
The anhydrous sodium sulfate and methanol 20mL of 5.0g, after shaking 2 minutes, stratification or 4000 turns/min centrifuge 5min, gained supernatant
Liquid is as sample treatment liquid；
（2）Detection：2mL derivatization reagents 01 are added in 5mL sample treatment liquids, the examination of 0.1mL derivatizations is added in shaking after five minutes
Agent 02 shakes 1 minute, stands 5 minutes, and the supernatant liquid color after observation is derivative shows sample if supernatant liquid shows red
In contain sulfa drugs, content is more than 100 μ g/kg；If the not aobvious red of supernatant liquid, using after chromatographic column processing two
Secondary detection, secondary detection, which operates, after chromatographic column processing is：
A, chromatographic column activates：2mL methanol and 5mL distilled water are sequentially added in chromatographic column, the speed of control chromatographic column liquid outflow
Degree is 1-2 drops/sec, discards efflux；
B, chromatography detection：Supernatant liquid is added in the chromatographic column after A step activation, 2mL deionized waters elution pillar is added, takes out
It is dry；Finally plus the elution of 0.8mL ethyl acetate, observation wash water color show to contain sulfanilamide (SN) in sample if eluent is aobvious red
Substance, content is more than 50 μ g/kg, under 100 μ g/kg.
2. rapid detection method according to claim 1, it is characterised in that：Step（2）Liquid is aobvious red specific at the middle and upper levels
For supernatant liquid displaing amaranth.
3. rapid detection method according to claim 1, it is characterised in that：The aobvious red of eluent is specially to wash in step B
De- liquid displaing amaranth.
4. rapid detection method according to claim 1, it is characterised in that：HLB reverse-phase chromatographies are loaded in the chromatographic column
The mass ratio of the mixture of filler and silica filler, HLB reverse-phase chromatographies filler and silica filler is 4：1.
5. rapid detection method according to claim 4, it is characterised in that：The HLB reverse-phase chromatographies filler average particle size：
40-60 μm, average pore size：80Å.
6. rapid detection method according to claim 4, it is characterised in that：The silica filler average particle size：40-60µ
M, average pore size：50Å.
7. rapid detection method according to claim 1, it is characterised in that：Step（2）Middle addition 2mL derivatization reagents 01
Regulation system pH value is 12 afterwards.
8. rapid detection method according to claim 1, it is characterised in that：01 specific ingredient of the derivatization reagent is matter
Measure the sodium carbonate liquor of concentration 5%.
9. rapid detection method according to claim 1, it is characterised in that：The derivatization reagent 02 specifically comprises：
The nitrous acid solution of mass concentration 5%, the aqueous solution of urea of mass concentration 5% and the beta naphthal ethanol solution of mass concentration 0.1% are pressed
According to 1:1:The mixture of 2 volume ratio.
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| CN2015104988838 | 2015-08-14 | ||
| CN201510498883.8A CN105116094A (en) | 2015-08-14 | 2015-08-14 | Fast detecting method for sulfonamide residues in shrimps |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106442510A (en) * | 2016-11-09 | 2017-02-22 | 百奥森（江苏）食品安全科技有限公司 | Sulfonamide test paper |
| CN107817306B (en) * | 2017-10-27 | 2020-06-19 | 中山出入境检验检疫局检验检疫技术中心 | Method for simultaneously detecting 64 veterinary drug residues in aquatic product |
| CN108107026B (en) * | 2017-11-30 | 2020-07-31 | 华南农业大学 | Method for identifying sulfonamides through chemical derivatization fluorescence-mass spectrometry |
| CN112611844B (en) * | 2021-01-11 | 2022-04-26 | 湛江国联水产开发股份有限公司 | Be applied to categorised sampling test device of shrimp shell and shrimp meat of raw shrimp production |
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| CN106093242A (en) | 2016-11-09 |
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