CN106596488A - Method for quick determination of sulfonamide residues in food - Google Patents

Method for quick determination of sulfonamide residues in food Download PDF

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Publication number
CN106596488A
CN106596488A CN201611151342.9A CN201611151342A CN106596488A CN 106596488 A CN106596488 A CN 106596488A CN 201611151342 A CN201611151342 A CN 201611151342A CN 106596488 A CN106596488 A CN 106596488A
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CN
China
Prior art keywords
sulfanilamide
food
enrichment phase
phase
sulfonamide
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Pending
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CN201611151342.9A
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Chinese (zh)
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蔡璇
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Individual
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Individual
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Priority to CN201611151342.9A priority Critical patent/CN106596488A/en
Publication of CN106596488A publication Critical patent/CN106596488A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6428Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material

Abstract

The invention discloses a method for quick determination of sulfonamide residues in food. The method includes the technological steps of a, weighing the weight of the food with the sulfonamide residues accurately, adding the weighed food with the sulfonamide residues into distilled water, mixing the food evenly prior to centrifugation, and taking out liquid supernatant; b, preparing a sulfonamide fluorescent derivative to obtain a standard substance enrichment phase; c, preparing a sample sulfonamide fluorescent derivative to obtain a sample enrichment phase; d, spotting the standard substance enrichment phase obtained in the step b and the sample enrichment phase obtained in the step c on a silica gel plate, observing fluorescence intensity of the standard substance enrichment phase and the sample enrichment phase under an ultraviolet lamp with ultraviolet light wavelength of 365 nm, and judging the sulfonamide residues in the food through comparison between the fluorescence intensity of the standard substance enrichment phase and that of the sample enrichment phase. The method is capable of detecting the sulfonamide residues in the food rapidly and effectively according to the above technological step design.

Description

Residual amount of sulfanilamide method for quick in a kind of food
Technical field
The present invention relates to residual amount of sulfanilamide quick detection side in food detection method technical field, more particularly to a kind of food Method.
Background technology
The animal-derived foods such as milk, interior product are generally abundant containing protein, fat, amino acid, carbohydrate, calcium, phosphorus, iron etc. Nutriment, as people's living standard is constantly improved, milk, the meat products proportion in the diet structure of resident It is increasing.
Wherein, sulfa drugs because its have the advantages that inexpensively, curative effect is high, short treating period, and is widely used in herding In industry production, for preventing and treating livestock and poultry pestilence.The a large amount of use of sulfa drugs causes it in most animals source food In have a residual, after the exceeded animal-derived food of the edible residual quantity of sulfonamide of people, health can be worked the mischief.
So, residual amount of sulfanilamide in food is detected and is just seemed and is highly desirable to.
The content of the invention
It is an object of the invention to provide residual amount of sulfanilamide method for quick in a kind of food, sulfanilamide (SN) residual in the food Amount method for quick can be detected fast and effeciently to residual amount of sulfanilamide in food.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
Residual amount of sulfanilamide method for quick in a kind of food, includes following processing step, specially:
A, the weight for accurately weighing sulfanilamide (SN) residual food product, and the sulfanilamide (SN) residual food product for weighing is added into distilled water, distill The consumption of water is 3-6ml/g, and mixing is centrifuged and takes out supernatant, standby;
B, prepare sulfanilamide (SN) fluorescent derivative:Configuration sulfanilamide (SN) concentration is the standard aqueous solution of 0.001-50mg/l, and toward above-mentioned standard Add quality percent by volume for the fluorescamine methanol solution of 0.05-0.1% in the aqueous solution, reaction 30-40 minutes stood under normal temperature, Then remove upper strata aqueous phase by the way that split-phase mode is centrifuged, to obtain standard items enrichment phase;
C, prepare sample sulfanilamide (SN) fluorescent derivative:The supernatant that step a is obtained is taken, and matter is added toward above-mentioned standard aqueous solution Amount percent by volume is the fluorescamine methanol solution of 0.05-0.1%, reaction 30-40 minutes is stood under normal temperature, then by centrifugation point Phase mode removes upper strata aqueous phase, to obtain example enrichment phase;
The example enrichment phase point sample that d, the standard items enrichment phase that step b is obtained and step c are obtained on silica gel plate, and Violet wavelength is observation caliber product enrichment phase, the fluorescence intensity of example enrichment phase under the ultraviolet light of 365nm, by comparing standard items The fluorescence intensity of the fluorescence intensity of enrichment phase and example enrichment phase to judge food in residual amount of sulfanilamide.
Wherein, in step b, the PH for adding the standard aqueous solution of fluorescamine methanol solution is 5-6.
Wherein, in step c, the PH for adding the supernatant of fluorescamine methanol solution is 5-6.
Beneficial effects of the present invention are:Residual amount of sulfanilamide method for quick in a kind of food of the present invention, its bag Following processing step is included:A, the weight for accurately weighing sulfanilamide (SN) residual food product, and by the sulfanilamide (SN) residual food product for weighing add to In distilled water, the consumption of distilled water is 3-6ml/g, and mixing is centrifuged and takes out supernatant, standby;B, prepare sulfanilamide (SN) fluorescent derivatization Thing:Configuration sulfanilamide (SN) concentration is the standard aqueous solution of 0.001-50mg/l, and quality volume hundred is added toward above-mentioned standard aqueous solution Divide the fluorescamine methanol solution than being 0.05-0.1%, reaction 30-40 minutes are stood under normal temperature, then gone by centrifugation split-phase mode Fall upper strata aqueous phase, to obtain standard items enrichment phase;C, prepare sample sulfanilamide (SN) fluorescent derivative:The supernatant that step a is obtained is taken, And add quality percent by volume for the fluorescamine methanol solution of 0.05-0.1% toward above-mentioned standard aqueous solution, stand under normal temperature anti- 30-40 minutes are answered, then removes upper strata aqueous phase by the way that split-phase mode is centrifuged, to obtain example enrichment phase;D, step b is obtained Standard items enrichment phase and step c obtain example enrichment phase point sample on silica gel plate, and violet wavelength for 365nm purple Observation caliber product enrichment phase, the fluorescence intensity of example enrichment phase under light lamp, by compare standard items enrichment phase fluorescence intensity with The fluorescence intensity of example enrichment phase to judge food in residual amount of sulfanilamide.Designed by above-mentioned processing step, the present invention can Fast and effeciently residual amount of sulfanilamide in food is detected.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
Residual amount of sulfanilamide method for quick in a kind of food, includes following processing step, specially:
A, the weight for accurately weighing sulfanilamide (SN) residual food product, and the sulfanilamide (SN) residual food product for weighing is added into distilled water, distill The consumption of water is 3-6ml/g, and mixing is centrifuged and takes out supernatant, standby;
B, prepare sulfanilamide (SN) fluorescent derivative:Configuration sulfanilamide (SN) concentration is the standard aqueous solution of 0.001-50mg/l, and toward above-mentioned standard Add quality percent by volume for the fluorescamine methanol solution of 0.05-0.1% in the aqueous solution, reaction 30-40 minutes stood under normal temperature, Then remove upper strata aqueous phase by the way that split-phase mode is centrifuged, to obtain standard items enrichment phase;
C, prepare sample sulfanilamide (SN) fluorescent derivative:The supernatant that step a is obtained is taken, and matter is added toward above-mentioned standard aqueous solution Amount percent by volume is the fluorescamine methanol solution of 0.05-0.1%, reaction 30-40 minutes is stood under normal temperature, then by centrifugation point Phase mode removes upper strata aqueous phase, to obtain example enrichment phase;
The example enrichment phase point sample that d, the standard items enrichment phase that step b is obtained and step c are obtained on silica gel plate, and Violet wavelength is observation caliber product enrichment phase, the fluorescence intensity of example enrichment phase under the ultraviolet light of 365nm, by comparing standard items The fluorescence intensity of the fluorescence intensity of enrichment phase and example enrichment phase to judge food in residual amount of sulfanilamide.
Wherein, in step b, the PH for adding the standard aqueous solution of fluorescamine methanol solution is 5-6;Likewise, the step In rapid c, the PH for adding the supernatant of fluorescamine methanol solution is 5-6.
Designed by above-mentioned processing step, the present invention can be detected fast and effeciently to residual amount of sulfanilamide in food.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's Thought, will change in specific embodiments and applications, and this specification content should not be construed as to the present invention Restriction.

Claims (3)

1. residual amount of sulfanilamide method for quick in a kind of food, it is characterised in that include following processing step, specially:
A, the weight for accurately weighing sulfanilamide (SN) residual food product, and the sulfanilamide (SN) residual food product for weighing is added into distilled water, distill The consumption of water is 3-6ml/g, and mixing is centrifuged and takes out supernatant, standby;
B, prepare sulfanilamide (SN) fluorescent derivative:Configuration sulfanilamide (SN) concentration is the standard aqueous solution of 0.001-50mg/l, and toward above-mentioned standard Add quality percent by volume for the fluorescamine methanol solution of 0.05-0.1% in the aqueous solution, reaction 30-40 minutes stood under normal temperature, Then remove upper strata aqueous phase by the way that split-phase mode is centrifuged, to obtain standard items enrichment phase;
C, prepare sample sulfanilamide (SN) fluorescent derivative:The supernatant that step a is obtained is taken, and matter is added toward above-mentioned standard aqueous solution Amount percent by volume is the fluorescamine methanol solution of 0.05-0.1%, reaction 30-40 minutes is stood under normal temperature, then by centrifugation point Phase mode removes upper strata aqueous phase, to obtain example enrichment phase;
The example enrichment phase point sample that d, the standard items enrichment phase that step b is obtained and step c are obtained on silica gel plate, and Violet wavelength is observation caliber product enrichment phase, the fluorescence intensity of example enrichment phase under the ultraviolet light of 365nm, by comparing standard items The fluorescence intensity of the fluorescence intensity of enrichment phase and example enrichment phase to judge food in residual amount of sulfanilamide.
2. residual amount of sulfanilamide method for quick in a kind of food according to claim 1, it is characterised in that:The step In b, the PH for adding the standard aqueous solution of fluorescamine methanol solution is 5-6.
3. residual amount of sulfanilamide method for quick in a kind of food according to claim 2, it is characterised in that:The step In c, the PH for adding the supernatant of fluorescamine methanol solution is 5-6.
CN201611151342.9A 2016-12-14 2016-12-14 Method for quick determination of sulfonamide residues in food Pending CN106596488A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611151342.9A CN106596488A (en) 2016-12-14 2016-12-14 Method for quick determination of sulfonamide residues in food

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611151342.9A CN106596488A (en) 2016-12-14 2016-12-14 Method for quick determination of sulfonamide residues in food

Publications (1)

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CN106596488A true CN106596488A (en) 2017-04-26

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1858232A (en) * 2006-03-27 2006-11-08 华中农业大学 Method for screening sulfanilamide medicine residue in edible animal tissue and reagent kit
US20090029349A1 (en) * 2002-09-27 2009-01-29 Siemens Medical Solutions Diagnostics Novel Applications of Acridinium Compounds and Derivatives in Homogeneous Assays
CN103760141A (en) * 2014-01-14 2014-04-30 昆明理工大学 Method for rapid detection of residual amount of sulfanilamide in food
CN105510428A (en) * 2016-01-27 2016-04-20 武汉矽感科技有限公司 Method for testing sulfamethoxazole in water by means of ion mobility spectrometer
WO2016151051A1 (en) * 2015-03-23 2016-09-29 Algipharma As Use of alginate oligomers and cftr modulators in the treatment of conditions associated with cftr dysfunction

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090029349A1 (en) * 2002-09-27 2009-01-29 Siemens Medical Solutions Diagnostics Novel Applications of Acridinium Compounds and Derivatives in Homogeneous Assays
CN1858232A (en) * 2006-03-27 2006-11-08 华中农业大学 Method for screening sulfanilamide medicine residue in edible animal tissue and reagent kit
CN103760141A (en) * 2014-01-14 2014-04-30 昆明理工大学 Method for rapid detection of residual amount of sulfanilamide in food
WO2016151051A1 (en) * 2015-03-23 2016-09-29 Algipharma As Use of alginate oligomers and cftr modulators in the treatment of conditions associated with cftr dysfunction
CN105510428A (en) * 2016-01-27 2016-04-20 武汉矽感科技有限公司 Method for testing sulfamethoxazole in water by means of ion mobility spectrometer

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