CN103760141B - A kind of method of residual amount of sulfanilamide in quick detection food - Google Patents
A kind of method of residual amount of sulfanilamide in quick detection food Download PDFInfo
- Publication number
- CN103760141B CN103760141B CN201410014635.7A CN201410014635A CN103760141B CN 103760141 B CN103760141 B CN 103760141B CN 201410014635 A CN201410014635 A CN 201410014635A CN 103760141 B CN103760141 B CN 103760141B
- Authority
- CN
- China
- Prior art keywords
- sulfanilamide
- residual amount
- sample
- food
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses the method for the residual amount of sulfanilamide in a kind of quick detection food, namely first sulfanilamide (SN) and fluorescamine generation derivatization reaction is adopted, with cloud point extraction, enrichment is carried out to derivative products again, on thin-layer silicon offset plate, point adds the on-gauge plate that sample enriched substance and sulfanilamide (SN) standard items are prepared into, under ultraviolet lamp, both fluorescence powers are compared, with the concentration range of sulfanilamide (SN) in judgement sample, for the mensuration of residual amount of sulfanilamide in food, method detects and is limited to 0.08 μ g/mL; Method of the present invention is simple to operate, consumption of organic solvent is little, detection sensitivity is high, detection time is short, high specificity, can effectively be separated with interfering material, it is a kind of easy, analytical approach fast and accurately, do not need large-scale instrument, only need configure miniature instrument equipment, be with a wide range of applications.
Description
Technical field
The invention belongs to technical field of food safety detection, relate to the detection method of residual sulfanilamide (SN) in food, particularly relate to the method for fluorescent derivatization and cloud point extraction.
Background technology
The animal-derived food such as milk, meat products is generally containing the nutriment that protein, fat, amino acid, carbohydrate, calcium, phosphorus, iron etc. are abundant, and along with improving constantly of living standards of the people, its proportion in the diet structure of resident is also increasing.Sulfa drugs has the advantages such as it is cheap, curative effect is high, short treating period because of it, is widely used in Animal husbandry production, for prevention and therapy livestock and poultry pestilence.It is residual that a large amount of uses of sulfa drugs cause it all to have in most animals derived food, and people can work the mischief to health after eating the animal-derived food that residual quantity of sulfonamide exceeds standard.In order to avoid consumer is subject to the harm of sulfa drug residue, there is the standard of the most high residue amount of corresponding rules and regulations in each state.European Union specifies that the residue limits of sulfa drugs in the food such as milk, meat is 100 μ gkg
1.
In prior art, the technology being applied to sulfa drug residue detection mainly contains microbiological method as TTC method, and immunoassay is as ELISA detection method, and chromatographic detection is as HPLC, GC method etc.Said method has his own strong points in detection precision etc., and some sensitivity is low, poor selectivity; Some operating process steps are comparatively loaded down with trivial details, and what have needs purchasing expensive instrument, but mostly exist and detect length consuming time, shortcoming that cost is high, bring inconvenience in concrete practical application.
Cloud point extraction method uses surfactant to extract the analysis thing in sample, and not using or only use a small amount of organic solvent, is a kind of environment amenable sample-pretreating method.Present invention employs NPE NP-7 is surfactant, it is unstressed configuration intensity under uviol lamp, can not the mensuration of jamming target material, the operating conditions of milder and comparatively high detection sensitivity, the feature such as quick, accurate is had compared with traditional extractant.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, the method of the residual amount of sulfanilamide in a kind of quick detection food is provided, this is a kind of effective novel using cloud point extraction system separation and concentration and detects the method for residual amount of sulfanilamide in food in conjunction with thin layer plate, while guarantee accuracy in detection and security, reduce testing cost, for quality supervision department provides accurately a kind of, convenient and swift, the assay method of qualitative, quantitative directly perceived.
The method of the residual amount of sulfanilamide that the present invention detects in food fast comprises the following steps:
(1) sample preparation: adding solvent containing sulfanilamide (SN) residual food product, mixing, centrifugal, take out supernatant, for subsequent use;
(2) formation of sulfanilamide (SN) fluorescent derivative and cloud point extraction: the standard aqueous solution of preparation sulfanilamide (SN) concentration 0.1 ~ 100mg/L, add the fluorescamine methanol solution that quality concentration of volume percent is 0.05% (w/v), by pH damping fluid regulation system to pH3 ~ 5, react 30min at normal temperatures, add non-ionic surfactant and inorganic salts, vortex mixed 2min, 20min is heated at 35 DEG C, centrifugal phase-splitting, remove upper strata aqueous phase, obtain standard items enrichment phase, wherein the addition of fluorescamine methanol solution is 0.1 ~ 0.5mL/5mL;
(3) formation of sample sulfanilamide (SN) fluorescent derivative and cloud point extraction: get step (1) gained supernatant, carry out derivatization reaction and cloud point extraction according to the condition described in step (2), obtain example enrichment phase;
(4) sulfanilamide (SN) content judges: the standard items enrichment phase of point sample step (2) and the example enrichment phase of step (3) on the thin-layer silicon offset plate of length >=3cm, after solvent volatilizes, under wavelength 365nm uviol lamp, both fluorescence powers are compared, sulfanilamide (SN) does not originally have fluorescence under uviol lamp, sulfanilamide (SN) after derivative is yellow green, by the yellow-green fluorescence strength ratio of the yellow-green fluorescence intensity of example enrichment phase and standard items enrichment phase comparatively, the concentration range of sulfanilamide (SN) is judged.
In step (1), sulfanilamide (SN) comprises one or several in sodium sulfadiazine SD, sulfamethyldiazine SM1, sulfamethazine SM2, sulfamethoxazole SMZ, sulphaguanidine SG; Solvent is the one in trichloroacetic acid, absolute ethyl alcohol, acetonitrile, methyl alcohol, water, and consumption is 0.08 ~ 0.4mL/mL or 0.1 ~ 5mL/g.
In step (2), pH damping fluid regulation system is the three acid buffering solution that boric acid, acetic acid and phosphoric acid are mixed with according to a conventional method; Non-ionic surfactant is NPE (7) ether, i.e. NP-7, and consumption is 0.01 ~ 0.2mL/5mL; Described inorganic salts comprise the one of sodium chloride, sodium sulphate, ammonium sulfate, ammonium chloride, and consumption is 0.05 ~ 0.3g/5mL.
Centrifugal condition described in the present invention is centrifugation time 10 ~ 20min, centrifugation rate 3000 ~ 6000r/min.
On the described thin-layer silicon offset plate of step (4), point sample amount is 30 μ L, and described example enrichment phase is identical with standard items enrichment phase point sample amount, and sampling point size is consistent, and diameter is at 0.2 ~ 0.6cm, and point sample divides and completes for 6 times.
Compared with the existing technology, the present invention has the following advantages or good effect:
1, because sulfa drugs itself does not have fluorescent absorption, so carry out mensuration again by derivative generation fluorescence sensitivity can be improved, material interference is reduced.The present invention utilizes sulfanilamide (SN) and fluorescamine reagent to derive, produce fluorescence, again by the enrichment sensitization of non-ionic surfactant, further raising fluorescence intensity, thus the high-sensitivity detection achieved sulfanilamide (SN), meet testing requirement during low residual amt, significantly improve system stability simultaneously, method detects and is limited to 0.08 μ g/mL, detect in application more feasible in reality, and NP-7, derivative reagent fluorescamine do not have fluorescence, so more not affecting fluorescence intensity under 365nm uviol lamp.
2, utilize thin-layer silicon offset plate point sample, fluorescence intensity compares, and method is easy, and consumption of organic solvent is little, highly sensitive.
3, method of operating is simple, and detection time is short, high specificity, can effectively be separated with interfering material, is a kind of easy, analytical approach fast and accurately, does not need large-scale instrument, only need configure miniature instrument equipment, be with a wide range of applications.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited to this.
embodiment 1:the present invention is utilized to carry out qualitative half-quantitative detection to sodium sulfadiazine residual quantity in milk
(1) compound concentration is respectively the sulphadiazine sodium standard solution 5mL of 0.1,1.0,10.0 and 100.0mg/L, add 0.1%(w/v respectively) fluorescamine methanol solution 0.2mL, the damping fluid regulation system made with boric acid, acetic acid and phosphorylated ligand is to pH5, after normal-temperature reaction 30min, add NP-70.02mL and sodium chloride 0.05g, vortex mixed 2min, 20min is heated at 35 DEG C, centrifugal 12min under rotating speed 4000r/min condition, now form upper strata aqueous phase and underlying surfaces activating agent enrichment phase, remove upper strata aqueous phase, obtain standard items enrichment phase; With methanol dilution to 0.4mL, interval 1.5cm on the thin-layer silicon offset plate of length 8cm, gets 30 μ L(each point sample 5 μ L, concurrent sample 6 times respectively) some plate, this series is as on-gauge plate, and totally four points, carry out fluorescence intensity for following examples and compare experiment.
(2) 5.0ml milk is got, add 2mL acetonitrile, mixing, centrifuging 10min under rotating speed 5000r/min condition, get supernatant water constant volume in 5mL, add 0.1%(w/v) fluorescamine methanol solution 0.2mL, with boric acid, the damping fluid regulation system that acetic acid and phosphorylated ligand are made is to pH5, after normal-temperature reaction 30min, add NP-70.02mL and sodium chloride 0.05g, vortex mixed 2min, 30min is heated at 35 DEG C, centrifugal 12min under rotating speed 4000r/min condition, now form upper strata aqueous phase and underlying surfaces activating agent enrichment phase, remove upper strata aqueous phase, obtain milk sample enrichment phase, with methanol dilution to 0.4mL, the thin-layer silicon offset plate of length 8cm adds sample solution 30 μ L(each point sample 5 μ L with amount respectively, concurrent sample 6 times), after sample and sulfanilamide (SN) enriched substance volatilize, obtain sample panel, step 1 is obtained on-gauge plate and sample panel is observed under wavelength 365nm uviol lamp, there is green fluorescence spot in example enrichment thing, relatively spot intensity, between 0.1-1.0mg/L, illustrate that in milk sample, sulfanilamide (SN) concentration is at 0.1 ~ 1mg/L.
embodiment 2:the present invention is utilized to carry out qualitative half-quantitative detection to sulfamethyldiazine residual quantity in pork
(1) with the step 1 of embodiment 1, difference is that the sulfanilamide (SN) used is sulfamethyldiazine;
(2) 0.5g pork is got, add 2mL methyl alcohol, mixing, centrifuging 10min under rotating speed 6000r/min condition, get supernatant water constant volume in 5mL, add 0.1%(w/v) fluorescamine methanol solution 0.3mL, with boric acid, the damping fluid regulation system that acetic acid and phosphorylated ligand are made is to pH5, after normal-temperature reaction 30min, add NP-70.05mL and sodium sulphate 0.1g, vortex mixed 2min, 30min is heated at 35 DEG C, centrifugal 12min under rotating speed 5000r/min condition, now form upper strata aqueous phase and underlying surfaces activating agent enrichment phase, remove upper strata aqueous phase, obtain pork example enrichment phase, with methanol dilution to 0.4mL, the thin-layer silicon offset plate of length 8cm adds sample solution 30 μ L(each point sample 5 μ L with amount respectively, concurrent sample 6 times), after sample and sulfanilamide (SN) enriched substance volatilize, obtain sample panel.Step 1 is obtained on-gauge plate and sample panel is observed under wavelength 365nm uviol lamp, having there is green fluorescence spot in example enrichment thing, compares spot intensity, do not observe fluorescence spot, to illustrate in pork sample that sulfamethyldiazine is residual and be less than 0.1mg/L.
embodiment 3:the present invention is utilized to carry out qualitative half-quantitative detection to sulfamethazine residual quantity in honey
Step 1: with the step 1 of embodiment 1, difference is that the sulfanilamide (SN) used is sulfamethazine;
Step 2: get 2.0g honey, add 5mL water, mixing, vortex 2.0min, filter, 3.0mL water is added again in filtrate, vortex 2.0min, centrifuging 15min under 3000r/min condition, get supernatant water constant volume in 5mL, add 0.1%(w/v) fluorescamine methanol solution 0.5mL, with boric acid, the damping fluid regulation system that acetic acid and phosphorylated ligand are made is to pH3, after normal-temperature reaction 30min, add NP-70.1mL and ammonium sulfate 0.2g, vortex mixed 2min, 30min is heated at 35 DEG C, centrifugal 20min under rotating speed 3000r/min condition, now form upper strata aqueous phase and underlying surfaces activating agent enrichment phase, remove upper strata aqueous phase, obtain honey sample enrichment phase, with methanol dilution to 0.4mL, the thin-layer silicon offset plate of length 8cm adds sample solution 30 μ L(each point sample 5 μ L with amount respectively, concurrent sample 6 times), after sample and sulfanilamide (SN) enriched substance volatilize, obtain sample panel.Step 1 is obtained on-gauge plate and sample panel is observed under wavelength 365nm uviol lamp, having there is green fluorescence spot in example enrichment thing, compares spot intensity, between 1-10mg/L, illustrates that in honey sample, sulfamethazine remains in 1 ~ 10mg/L.
embodiment 4:the present invention is utilized to carry out qualitative half-quantitative detection to sulfamethoxazole residual quantity in egg
Step 1: with the step 1 of embodiment 1, difference is that the sulfanilamide (SN) used is sulfamethoxazole;
Step 2: get the egg that 2.0g stirs, add 5mL acetonitrile, mixing, centrifuging 15min under rotating speed 6000r/min condition, get supernatant water constant volume in 5mL, add 0.1%(w/v) fluorescamine methanol solution 0.2mL, with boric acid, the damping fluid regulation system that acetic acid and phosphorylated ligand are made is to pH4, after normal-temperature reaction 30min, add NP-70.2mL and ammonium chloride 0.3g, vortex mixed 2min, 30min is heated at 35 DEG C, centrifugal 12min under rotating speed 4500r/min condition, now form upper strata aqueous phase and underlying surfaces activating agent enrichment phase, remove upper strata aqueous phase, obtain egg sample enrichment phase, with methanol dilution to 0.4mL, the thin-layer silicon offset plate of length 8cm adds sample solution 30 μ L(each point sample 5 μ L with amount respectively, concurrent sample 6 times), after sample and sulfanilamide (SN) enriched substance volatilize, obtain sample panel, step 1 is obtained on-gauge plate and sample panel is observed under wavelength 365nm uviol lamp, having there is green fluorescence spot in example enrichment thing, compares spot intensity, between 0.1 ~ 1mg/L, illustrates that in egg sample, sulfamethoxazole remains in 0.1 ~ 1mg/L.
Confirmatory experiment, under identical disposal route, treatment conditions, the testing result of different detecting device is as follows:
Claims (5)
1. detect a method for the residual amount of sulfanilamide in food fast, it is characterized in that comprising the following steps:
(1) sample preparation: adding solvent containing sulfanilamide (SN) residual food product, mixing, centrifugal, take out supernatant, for subsequent use;
(2) formation of sulfanilamide (SN) fluorescent derivative and cloud point extraction: the standard aqueous solution of preparation sulfanilamide (SN) concentration 0.1 ~ 100mg/L, add the fluorescamine methanol solution that quality concentration of volume percent is 0.05-0.1%, by pH damping fluid regulation system to pH3 ~ 5, react 30min at normal temperatures, add non-ionic surfactant and inorganic salts, vortex mixed 2min, 20min is heated at 35 DEG C, centrifugal phase-splitting, remove upper strata aqueous phase, obtain standard items enrichment phase, wherein the addition of fluorescamine methanol solution is 0.1 ~ 0.5mL/5mL;
(3) formation of sample sulfanilamide (SN) fluorescent derivative and cloud point extraction: get step (1) gained supernatant water constant volume, carry out derivatization reaction and cloud point extraction according to the condition described in step (2), obtain example enrichment phase;
(4) sulfanilamide (SN) content judges: the standard items enrichment phase of point sample step (2) and the example enrichment phase of step (3) on thin-layer silicon offset plate, after solvent volatilizes, under wavelength 365nm uviol lamp, both fluorescence powers are compared, sulfanilamide (SN) after derivative is yellow green, by the yellow-green fluorescence strength ratio of the yellow-green fluorescence intensity of example enrichment phase and standard items enrichment phase comparatively, the concentration range of sulfanilamide (SN) is judged;
Described non-ionic surfactant is NPE (7) ether, and consumption is 0.01 ~ 0.2mL/5mL;
Described inorganic salts comprise in sodium chloride, sodium sulphate, ammonium sulfate, ammonium chloride a kind of, and consumption is 0.05 ~ 0.3g/5mL.
2. detect the method for the residual amount of sulfanilamide in food according to claim 1 fast, it is characterized in that: sulfanilamide (SN) is one or several in sodium sulfadiazine SD, sulfamethyldiazine SM1, sulfamethazine SM2, sulfamethoxazole SMZ, sulphaguanidine SG.
3. detect the method for the residual amount of sulfanilamide in food according to claim 1 fast, it is characterized in that: solvent is the one in trichloroacetic acid, absolute ethyl alcohol, acetonitrile, methyl alcohol, water, consumption is 0.08 ~ 0.4mL/mL or 0.1 ~ 5mL/g.
4. detect the method for the residual amount of sulfanilamide in food according to claim 1 fast, it is characterized in that: the three acid buffering solution that pH damping fluid regulation system is boric acid, acetic acid, phosphorylated ligand are made.
5. detect the method for the residual amount of sulfanilamide in food according to claim 1 fast, it is characterized in that: centrifugal condition is centrifugation time 10 ~ 20min, centrifugation rate 3000 ~ 6000r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410014635.7A CN103760141B (en) | 2014-01-14 | 2014-01-14 | A kind of method of residual amount of sulfanilamide in quick detection food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410014635.7A CN103760141B (en) | 2014-01-14 | 2014-01-14 | A kind of method of residual amount of sulfanilamide in quick detection food |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103760141A CN103760141A (en) | 2014-04-30 |
| CN103760141B true CN103760141B (en) | 2016-03-30 |
Family
ID=50527416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410014635.7A Active CN103760141B (en) | 2014-01-14 | 2014-01-14 | A kind of method of residual amount of sulfanilamide in quick detection food |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103760141B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116094A (en) * | 2015-08-14 | 2015-12-02 | 舟山出入境检验检疫局综合技术服务中心 | Fast detecting method for sulfonamide residues in shrimps |
| CN106546693B (en) * | 2016-10-25 | 2018-05-08 | 烟台大学 | A kind of method of portable imaging method detection sulfa drug residue and application thereof |
| CN106596488A (en) * | 2016-12-14 | 2017-04-26 | 蔡璇 | Method for quick determination of sulfonamide residues in food |
| CN106770793A (en) * | 2017-01-20 | 2017-05-31 | 烟台出入境检验检疫局检验检疫技术中心 | The method that QNS in breast or dairy products is detected using cloud point extraction liquid chromatography tandem mass spectrometry |
| CN106770792B (en) * | 2017-01-20 | 2019-07-16 | 烟台出入境检验检疫局检验检疫技术中心 | Using the method for beta-receptor stimulant medicine in cloud point extraction-liquid chromatography tandem mass spectrometry detection cream or dairy products |
| CN108107026B (en) * | 2017-11-30 | 2020-07-31 | 华南农业大学 | Method for identifying sulfonamides through chemical derivatization fluorescence-mass spectrometry |
| CN109916873B (en) * | 2019-04-11 | 2021-12-24 | 江西农业大学 | Method for simultaneously detecting two antibiotic residues in water by time-resolved synchronous fluorescence method |
| CN112082846B (en) * | 2020-09-16 | 2022-07-19 | 中南林业科技大学 | Environment-friendly pretreatment method for sulfamethazine detection sample in muscle |
| CN115014890B (en) * | 2022-05-18 | 2023-06-02 | 深圳职业技术学院 | Sample processing method and nitrofuran metabolite determination method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435823A (en) * | 2007-11-12 | 2009-05-20 | 无锡中德伯尔生物技术有限公司 | Fluorescent micro-ball immune chromatography test paper strip for detecting residual animal medicine and preparing method thereof |
| CN102928417A (en) * | 2011-08-09 | 2013-02-13 | 北京勤邦生物技术有限公司 | Magnetic particle chemiluminescence kit for detecting sulfanilamide drugs, and applications thereof |
| CN103045869A (en) * | 2012-12-27 | 2013-04-17 | 北京大学 | Method for enriching uranium and thorium from water phase by using cloud point extraction technology |
-
2014
- 2014-01-14 CN CN201410014635.7A patent/CN103760141B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435823A (en) * | 2007-11-12 | 2009-05-20 | 无锡中德伯尔生物技术有限公司 | Fluorescent micro-ball immune chromatography test paper strip for detecting residual animal medicine and preparing method thereof |
| CN102928417A (en) * | 2011-08-09 | 2013-02-13 | 北京勤邦生物技术有限公司 | Magnetic particle chemiluminescence kit for detecting sulfanilamide drugs, and applications thereof |
| CN103045869A (en) * | 2012-12-27 | 2013-04-17 | 北京大学 | Method for enriching uranium and thorium from water phase by using cloud point extraction technology |
Non-Patent Citations (2)
| Title |
|---|
| Ultrasound-assisted cloud point extraction for the determination of sulfonamides in honey samples by fluorescence spectrophotometry;Fang Yu等;《Analytical Methods》;20130409;第24卷(第5期);第3921页第1栏第2段-第2栏第3段，第3921页第2栏倒数第3段，第3925页第1栏第1段及图2，图5 * |
| 层析扫描与药物分析;邵玉麟;《药学通报》;19781231(第2期);第76页第1栏第2段，第2栏第4段，第77页第1栏第4段，第79页第1栏第1-3段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103760141A (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103760141B (en) | A kind of method of residual amount of sulfanilamide in quick detection food | |
| Li et al. | Toxins in mussels (Mytilus galloprovincialis) associated with diarrhetic shellfish poisoning episodes in China | |
| Stoloff et al. | A multimycotoxin detection method for aflatoxins, ochratoxins, zearalenone, sterigmatocystin, and patulin | |
| CN102175784B (en) | Method for synchronously detecting 54 medicament residues in pork by virtue of solid phase extraction-liquid chromatogram-mass spectrum/mass spectrometry | |
| Liu et al. | Determination of triazine herbicides in milk by cloud point extraction and high-performance liquid chromatography | |
| Zhou et al. | Analysis of tetracyclines in chicken tissues and dung using LC–MS coupled with ultrasound-assisted enzymatic hydrolysis | |
| CN105021756B (en) | Amantadine, rimantadine, ribavirin, the multi-joint detection method of Moroxydine residual in a kind of fowl egg | |
| CN103091314B (en) | Rapid detection method for water-soluble azo dyes in foods | |
| CN102033102A (en) | Method for screening beta-lactamase antibiotic decomposing agent in dairy products by high flux matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) | |
| CN101830980B (en) | Chlorothalonil antigen, antibody preparation method and residual chlorothalonil ELISA (Enzyme-Linked Lmmuno Sorbent Assay) detection method | |
| Hassouan et al. | Multiresidue method for simultaneous determination of quinolone antibacterials in pig kidney samples by liquid chromatography with fluorescence detection | |
| CN105445259A (en) | Method for quickly detecting clenbuterol based on functionalized gold nanoparticles | |
| Shi et al. | Simultaneous determination of 14 nitroimidazoles using thin-layer chromatography combined with surface-enhanced Raman spectroscopy (TLC-SERS) | |
| Johnson et al. | Quantification of saxitoxin and neosaxitoxin in human urine utilizing isotope dilution tandem mass spectrometry | |
| CN102875512B (en) | Preparation method of anticoagulant raticide brodifacoum hapten and holoantigen | |
| ZHANG et al. | A portable photoelectric sensor based on colloidal gold immunochromatographic strips for rapid determination of clenbuterol in pig urine | |
| Ebisuda et al. | Lipid-soluble and water-soluble arsenic compounds in blubber of ringed seal (Pusa hispida) | |
| CN104311659A (en) | Multi-cluster antigen and wide-spectrum specific antibody of beta-adrenoceptor agonists and application of multi-cluster antigen and wide-spectrum specific antibody | |
| CN104387467A (en) | Detection kit and detection paper for Beta-adrenergic receptor stimulant multiresidue detection | |
| CN103616376A (en) | Method for detecting steroidal anti-inflammation drugs in Chinese patent medicines and health-care products | |
| Grotti et al. | Arsenic species in certified reference material MURST-ISS-A2 (Antarctic krill) | |
| CN106543284A (en) | A kind of preparation method and application of crotoxyphos, Carbicron and omethoate antibody | |
| CN103314973B (en) | Method for extracting anti-artemia active ingredients from styela canopus | |
| CN102692384B (en) | Detection method of gizzerosine in fish meal | |
| CN104215491A (en) | Method for extracting and detecting heme from plants |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |