CN107957417A - The detection reagent and its assay method of sulfur dioxide in food concentration - Google Patents

The detection reagent and its assay method of sulfur dioxide in food concentration Download PDF

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Publication number
CN107957417A
CN107957417A CN201610900005.9A CN201610900005A CN107957417A CN 107957417 A CN107957417 A CN 107957417A CN 201610900005 A CN201610900005 A CN 201610900005A CN 107957417 A CN107957417 A CN 107957417A
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China
Prior art keywords
detection reagent
sulfur dioxide
parts
weight
food concentration
Prior art date
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Pending
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CN201610900005.9A
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Chinese (zh)
Inventor
葛平兰
唐华荣
赵恒�
张军强
程艳
冯振军
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Simon Biotechnology Co Ltd Shandong
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Simon Biotechnology Co Ltd Shandong
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Priority to CN201610900005.9A priority Critical patent/CN107957417A/en
Publication of CN107957417A publication Critical patent/CN107957417A/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
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • 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
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/775Indicator and selective membrane

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a kind of detection reagent and its assay method of sulfur dioxide in food concentration, belong to analysis and survey control technology field.The detection reagent of the sulfur dioxide in food concentration of the present invention includes the component of following parts by weight:000 5000 parts of 15 parts of dithio-bis-nitrobenzoic acid (DTNB), 15 parts of sodium acid carbonate and phosphate buffer 1.The method being detected in the present invention using above-mentioned detection reagent includes the use of sample and distilled water configuration sample aqueous solution;Measure group and control group are set in ELISA Plate detection hole;The detection reagent configured is added separately to measure group and the control group of ELISA Plate detection hole in step 2.Detection reagent raw material of the present invention composition is simple, it is easy to operate it is time saving, cheap, linear relationship is good, detection sensitivity higher, minimum detection limit can reach 0.2mg/kg.

Description

The detection reagent and its assay method of sulfur dioxide in food concentration
Technical field
The present invention relates to analysis and survey control technology field, a kind of detection of sulfur dioxide in food concentration is particularly related to Reagent and its assay method.
Background technology
Sulfur dioxide is applied in food processing process, is usually deposited in the form of sequestered and the sulfite ion of mating type Anti-corrosion, bleaching, fresh-keeping effect can be being played, is extending the shelf-life of product.But human body takes in sulfur dioxide for a long time can destroy dimension Raw element B1, can cause a variety of disease harm such as function of intestinal canal disorder, compromised liver function, polyneuritis and bone marrow suppression. China using sulfur dioxide in food to being made that limitation regulation.The method master of sulfur dioxide residue in detection food at present If pararosaniline hydrochloridc colorimetric method and distillation titration.Both detection reagent methods all contain in reagent raw material to be made Into the heavy metal component of secondary pollution, and preparation of reagents and it is complicated time-consuming, the sensitivity of detection is 1mg/kg.For full The demand of toe ring guarantor, quick detection and trace detection, also have certain limitation.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of detection reagent and its measure of sulfur dioxide in food concentration Method.The present invention avoids the introducing of harmful heavy metal component, simplifies by changing on detection reagent component and colour developing principle Reagent forms and operating procedure, and realizes the detection sensitivity of 0.2mg/kg.
In order to solve the above technical problems, present invention offer technical solution is as follows:
A kind of detection reagent of sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):1-8 parts by weight;
Sodium acid carbonate:1-8 parts by weight;
Biological buffer:800-6000 parts by weight.
Preferably, the detection reagent of the sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):1-5 parts by weight;
Sodium acid carbonate:1-5 parts by weight;
Biological buffer:1000-5000 parts by weight.
Wherein, the biological buffer is phosphate buffer.
On the other hand, there is provided a kind of method that detection reagent of above-mentioned sulfur dioxide in food concentration is measured, including Following steps:
Step 1:Use sample and distilled water configuration sample aqueous solution;
Step 2:Measure group and control group are set in ELISA Plate detection hole, and the measure group adds the sample that step 1 obtains Product aqueous solution, the control group add the isometric distilled water of the sample aqueous solution obtained with step 1;
Step 3:The detection reagent configured is added separately to measure group and the control of ELISA Plate detection hole in step 2 Group, is uniformly mixed and places 3-10 minutes;
Step 4:The absorption values of measure group and control group under wavelength 412nm in read step 3.
Wherein, the sample in the step 1 is solid sample or fluid sample.
Further, after the solid sample pulverization process 1 is pressed with distilled water:2 parts by weight uniformly mix and take supernatant Liquid;The fluid sample presses 1 with distilled water:4 volume ratio uniformly mixes.
Volume ratio for the detection reagent in the step 3 and measure group and control group is 1:6-10.
Wherein, for the absorption values of measure group and control group in the step 4, microplate reader or light splitting light can be passed through Instrument is spent to read.
Further, the absorption values of the measure group in step 4 are denoted as A1, the extinction number of degrees numerical value note of control group Make A0;Calculate the titanium dioxide of the measure group respectively according to formula content of sulfur dioxide=extension rate × coefficient × (A1-A0) Sulfur content.
The invention has the advantages that:
It is of the invention can overcome the deficiencies in the prior art, avoid use toxic heavy metal component, it is and same before such as four mercury chloride The detection method of class is compared, and the detection reagent raw material composition of sulfur dioxide in food concentration provided by the invention is simple, and reagent Composition is only a kind of mix ingredients, when being measured using this detection reagent, time saving, cheap, line easy to operate Sexual intercourse is good, and detection sensitivity higher, and the minimum detection limit of testing result can reach 0.2mg/kg, can meet micro- in food Measure the detection demand of sulfur dioxide.
Embodiment
The present invention provides a kind of detection reagent and its assay method of sulfur dioxide in food concentration, to make the present invention's Purpose, technical solution and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that this place is retouched The specific embodiment stated only to explain the present invention, is not intended to limit the present invention.
Embodiment 1
The detection reagent of sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):1 parts by weight;
Sodium acid carbonate:1 parts by weight;
Biological buffer:800 parts by weight.
Wherein, the biological buffer is phosphate buffer.
Embodiment 2
The detection reagent of sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):8 parts by weight;
Sodium acid carbonate:8 parts by weight;
Biological buffer:6000 parts by weight.
Wherein, the biological buffer is phosphate buffer.
Embodiment 3
The detection reagent of sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):1 parts by weight;
Sodium acid carbonate:1 parts by weight;
Biological buffer:1000 parts by weight.
Wherein, the biological buffer is phosphate buffer.
Embodiment 4
The detection reagent of sulfur dioxide in food concentration, includes the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):5 parts by weight;
Sodium acid carbonate:5 parts by weight;
Biological buffer:5000 parts by weight.
Wherein, the biological buffer is phosphate buffer.
As can be seen from the above embodiments, the detection reagent of sulfur dioxide in food concentration provided by the invention avoids using Toxic heavy metal component, such as four mercury chloride, and reagent composition is only a kind of mix ingredients, raw material composition is simple.
A kind of corresponding assay method is also provided for the detection reagent of sulfur dioxide in food concentration provided by the invention, It is specific as follows:
Embodiment 5
Step 1:Use sample and distilled water configuration sample aqueous solution;Sample can be solid sample or fluid sample, Solid kind sample is shredded or ground as far as possible;For solid sample, 1 is pressed with distilled water after usual pulverization process:2 parts by weight are equal Even mixing, ultrasonic vibration 5~10 minutes, need to filter to take filtrate when supernatant is unclear, spare as sample extracting solution;For liquid Sample, usually presses 1 with distilled water:4 volume ratio uniformly mixes.
Step 2:Measure group and control group are set in ELISA Plate detection hole, the perpendicular row in the left side first are added into 250 μ L distillations Water compares group, and the 250ul sample extraction liquid that remaining each detection hole adds same volume makees measure group;
Step 3:Be added separately to after the detection reagent configured is shaken up ELISA Plate detection hole in step 2 measure group and Control group, 30 μ L are added per hole, and the surrounding concussion of tapping ELISA Plate is placed 3-10 minutes after mixing;
Step 4:The absorption values of measure group and control group under wavelength 412nm in read step 3;In step 4 The absorption values of the measure group are denoted as A1, and the extinction number of degrees numerical value of control group is denoted as A0;The extinction of measure group and control group Number of degrees value can be read by microplate reader or spectrophotometer.
Finally the measure can be calculated respectively according to formula content of sulfur dioxide=extension rate × coefficient × (A1-A0) The content of sulfur dioxide of group.
Solid sample and fluid sample with certain content sulfur dioxide are prepared respectively in advance, for judging after measure The accuracy of the detection method of the present invention, i.e., accurately prepare certain density solution as sample, then using in embodiment 1-4 Detection reagent and the method and step of embodiment 5 complete measure, the control group of every group of test all uses distilled water.By the extinction number of degrees Value substitutes into formula:Content of sulfur dioxide=extension rate × coefficient × (A1-A0).
Wherein, content of sulfur dioxide (mg/kg)=extension rate × 7.001 × (A1-A0) in solid
Content of sulfur dioxide (mg/kg)=extension rate × 7.001 × (A1-A0) in liquid
To the test result analysis of solid sample and fluid sample, detection reagent of the present invention and detection are found Method, can in accurate determination sample trace sulfur dioxide concentration, the minimum detection limit of testing result can reach 0.2mg/kg.And solid sample grinding and sonic oscillation pre-treatment are more abundant, measurement result is closer to actual value.Testing principle Reacted for inferior sulfate radical and two thio-bis--nitrobenzoic acids (DTNB), generation 2- nitro -5- thiobenzoates (NTB), There is maximum absorption band at 412nm, the concentration and color reaction degree of inferior sulfate radical are in a linear relationship.It is repeatedly real by applicant Test, this method has higher reliability, can be widely used in the inspection for needing to detect trace sulfur dioxide concentration in food Field.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope that this specification is recorded all is considered to be.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art For, without departing from the principles of the present invention, some improvements and modifications can also be made, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (9)

1. a kind of detection reagent of sulfur dioxide in food concentration, it is characterised in that include the component of following parts by weight:
Two thio-bis--nitrobenzoic acids (DTNB):1-8 parts by weight;
Sodium acid carbonate:1-8 parts by weight;
Biological buffer:800-6000 parts by weight.
2. the detection reagent of sulfur dioxide in food concentration according to claim 1, it is characterised in that including following weight The component of part:
Two thio-bis--nitrobenzoic acids (DTNB):1-5 parts by weight;
Sodium acid carbonate:1-5 parts by weight;
Biological buffer:1000-5000 parts by weight.
3. the detection reagent of sulfur dioxide in food concentration according to claim 2, it is characterised in that the biological buffer Liquid is phosphate buffer.
4. the method that the detection reagent of any sulfur dioxide in food concentration of claim 1-3 is measured, its feature It is, comprises the following steps:
Step 1:Use sample and distilled water configuration sample aqueous solution;
Step 2:Measure group and control group are set in ELISA Plate detection hole, and the measure group adds the sample water that step 1 obtains Solution, the control group add isometric distilled water;
Step 3:The detection reagent configured is added separately to the measure group and control group of ELISA Plate detection hole in step 2, is mixed Close and uniformly place 3-10 minutes;
Step 4:The absorption values of measure group and control group under wavelength 412nm in read step 3.
5. the method that the detection reagent of sulfur dioxide in food concentration according to claim 4 is measured, its feature exist In the sample in the step 1 is solid sample or fluid sample.
6. the method that the detection reagent of sulfur dioxide in food concentration according to claim 5 is measured, its feature exist In with distilled water by 1 after the solid sample pulverization process:2 parts by weight uniformly mix and take supernatant;The fluid sample 1 is pressed with distilled water:4 volume ratio uniformly mixes.
7. the method that the detection reagent of sulfur dioxide in food concentration according to claim 4 is measured, its feature exist In detection reagent and measure group and the volume ratio of control group in the step 3 are 1:6-10.
8. the method that the detection reagent of sulfur dioxide in food concentration according to claim 4 is measured, its feature exist In the absorption values of measure group and control group are read by microplate reader or spectrophotometer in the step 4.
9. the method that the detection reagent of sulfur dioxide in food concentration according to claim 8 is measured, its feature exist In the absorption values of the measure group are denoted as A1, and the extinction number of degrees numerical value of control group is denoted as A0;The titanium dioxide of the measure group Sulfur content=extension rate × coefficient × (A1-A0).
CN201610900005.9A 2016-10-17 2016-10-17 The detection reagent and its assay method of sulfur dioxide in food concentration Pending CN107957417A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105021601A (en) * 2015-06-24 2015-11-04 西南大学 Food sulfur dioxide content determination method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105021601A (en) * 2015-06-24 2015-11-04 西南大学 Food sulfur dioxide content determination method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
RAY E. HUMPHREY, ET AL.: "Spectrophotometric Determination of Sulfite with 4,4‘-Dithiodipyridine and 5,5’-Dithiobis- (2- Nitrobenzoic Acid)", 《ANALYTICAL CHEMISTRY》 *
YONGJIE LI ET AL: "Simple methods for rapid determination of sulfite in food products", 《FOOD CONTROL》 *
罗兰主编: "《植物化学保护试验指导》", 31 October 2015, 中国农业大学出版社 *

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Application publication date: 20180424