CN107462643A - The assay method of thiourea dioxide in a kind of food additives - Google Patents
The assay method of thiourea dioxide in a kind of food additives Download PDFInfo
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- CN107462643A CN107462643A CN201710611223.5A CN201710611223A CN107462643A CN 107462643 A CN107462643 A CN 107462643A CN 201710611223 A CN201710611223 A CN 201710611223A CN 107462643 A CN107462643 A CN 107462643A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a kind of assay method of thiourea dioxide in food additives.The assay method comprises the following steps：1) extract：0.1g food additives are weighed, acetum dissolving is added, ice-water bath ultrasonic extraction, is settled to 100mL；2) sample solution is prepared：Stand step 1) and obtain solution, take supernatant 1mL, add acetonitrile and be settled to 10mL, through 0.45 μm of membrane filtration, gained subsequent filtrate is sample solution；3) detect：Sample solution is detected using high performance liquid chromatography；4) confirm：Confirmed using high performance liquid chromatography MS.The method simple and fast of the present invention, the qualitative and quantitative determination of thiourea dioxide suitable for the food additives for declaring to have the effects such as anti-oxidant, anti-corrosion, fresh-keeping, light tone color protection, increasing muscle, and positive confirmation.
Description
Technical field
The present invention relates to a kind of assay method of thiourea dioxide in food additives.
Background technology
Thiourea dioxide also known as thiourea peroxide, alias are FAS (TDO), and the product are that important industry becomes more meticulous
Product, should print and dye extensively in the industry, papermaking, the reduction remover of fiber industry etc., bleaching stripping agent；High polymer synthesis industry
Catalyst, stabilizer and multifunctional assistant；Reducing agent in organic synthesis；Sensitizer, the antioxidant of photosensitive material.
There is the bleaching that thiourea dioxide is replaced food bleaching agent to be used for food by illegal retailer, so as to improve the outward appearance of food
And mouthfeel.Headache, nausea, oral cavity and gastric irritation can be caused after edible thiourea dioxide, but it is domestic still not on food at present
The relevant criterion of middle thiourea dioxide detection method, therefore, establishing the efficiently and accurately detection method of thiourea dioxide in food is
An urgent demand to ensure food safety.
The industrial goods of thiourea dioxide can pass through the classical detection method such as iodimetric titration, potassium dichromate method and neutralization titration
To detect its purity and content.But thiourea dioxide is used as bleaching agent, most of during bleaching to have decomposed, it is being eaten
Residual quantity in product is trace, and is easily disturbed by other matrix, and above method sensitivity can not reach the requirement of trace detection.
The content of the invention
It is an object of the invention to provide a kind of assay method of thiourea dioxide in food additives.
The technical solution used in the present invention is：
The assay method of thiourea dioxide, comprises the following steps in a kind of food additives：
1) extract：0.1g food additives are weighed, acetum dissolving is added, ice-water bath ultrasonic extraction, is settled to
100mL；
2) sample solution is prepared：
A, stand step 1) and obtain solution, take supernatant 1mL, 10mL is settled to acetonitrile, through 0.45 μm of membrane filtration, institute
It is sample solution a to obtain subsequent filtrate；
B, stand step 1) and obtain solution, take 0.01mL, 10mL is settled to acetum, be made into middle storing solution；Take
Middle storing solution 1mL, 10mL is settled to acetonitrile, and through 0.45 μm of membrane filtration, gained subsequent filtrate is sample solution b；
3) detect：Sample solution a is detected using high performance liquid chromatography；
4) confirm：Positive confirmation is carried out to sample solution b using tablets by HPLC-MS.
The volumetric concentration of acetum is 0.05%.
In step 1), the time of ultrasonic extraction is 8~12min.
Instrument used in high performance liquid chromatography is the high-efficient liquid phase color with PDAD or UV-detector
Spectrometer.
The testing conditions of step 3) are as follows：
Chromatographic column：HILIC posts, 150mm × 4.6mm, 2.7 μm；
Flow velocity：0.8~1.2mL/min；
Sample size：10μL；
Column temperature：28~32 DEG C；
PDAD wave-length coverage：190~600nm；Or UV-detector Detection wavelength：284nm.
The testing conditions of step 4) are as follows：
Chromatographic column：HILIC posts, 100mm × 2.1mm, 1.7 μm；
Flow velocity：0.2~0.3mL/min；
Sample size：5μL；
Column temperature：38~42 DEG C；
Ion gun：Electric spray ion source；
Scan pattern：Positive ion mode；
Detection pattern：More reaction detection patterns, second order spectrum full scan.
The beneficial effects of the invention are as follows：
The method simple and fast of the present invention, suitable for declaring to have anti-oxidant, anti-corrosion, fresh-keeping, light tone color protection, increasing the effect such as muscle
Food additives in thiourea dioxide qualitative and quantitative determination, and positive confirmation.
Brief description of the drawings
Fig. 1 is the liquid chromatogram of thiourea dioxide reference material；
Fig. 2 is the spectrogram of thiourea dioxide reference material；
Fig. 3 is application examples bleaching agent A spectrogram；
Fig. 4 is application examples bleaching agent B spectrogram；
Fig. 5 is that the MRM of thiourea dioxide reference material schemes；
Fig. 6 is that the two level of thiourea dioxide reference material traces designs entirely；
The MRM that Fig. 7 is application examples bleaching agent A schemes；
The two level that Fig. 8 is application examples bleaching agent A traces designs entirely；
The MRM that Fig. 9 is application examples bleaching agent B schemes；
The two level that Figure 10 is application examples bleaching agent B traces designs entirely.
Embodiment
The assay method of thiourea dioxide, comprises the following steps in a kind of food additives：
1) extract：0.1g food additives are weighed, acetum dissolving is added, ice-water bath ultrasonic extraction, is settled to
100mL；
2) sample solution is prepared：
A, stand step 1) and obtain solution, take supernatant 1mL, 10mL is settled to acetonitrile, through 0.45 μm of membrane filtration, institute
It is sample solution a to obtain subsequent filtrate；
B, stand step 1) and obtain solution, take 0.01mL, 10mL is settled to acetum, be made into middle storing solution；Take
Middle storing solution 1mL, 10mL is settled to acetonitrile, and through 0.45 μm of membrane filtration, gained subsequent filtrate is sample solution b；
3) detect：Sample solution a is detected using high performance liquid chromatography；
4) confirm：Positive confirmation is carried out to sample solution b using tablets by HPLC-MS.
Preferably, the volumetric concentration of acetum is 0.05%.
Preferably, in step 1), the time of ultrasonic extraction is 8~12min；It is further preferred that in step 1), ultrasound carries
The time taken is 10min.
Preferably, the instrument used in high performance liquid chromatography is efficient with PDAD or UV-detector
Liquid chromatograph.
Preferably, the testing conditions of step 3) are as follows：
Chromatographic column：HILIC (hydrophilic Interaction Chromatography) post, 150mm × 4.6mm, 2.7 μm；
Flow velocity：0.8~1.2mL/min；
Sample size：10μL；
Column temperature：28~32 DEG C；
PDAD wave-length coverage：190~600nm；Or UV-detector Detection wavelength：284nm.
It is further preferred that the testing conditions of step 3) are as follows：
Chromatographic column：HILIC posts, 150mm × 4.6mm, 2.7 μm；
Flow velocity：1.0mL/min；
Mobile phase：The volume ratio of acetonitrile/water, wherein acetonitrile and water is 9：1；
Sample size：10μL；
Column temperature：30℃；
PDAD wave-length coverage：190~600nm；Or UV-detector Detection wavelength：284nm.
Preferably, step 3) condition of gradient elution is as follows：
Preferably, the testing conditions of step 4) are as follows：
Chromatographic column：HILIC posts, 100mm × 2.1mm, 1.7 μm；
Flow velocity：0.2~0.3mL/min；
Sample size：5μL；
Column temperature：38~42 DEG C；
Ion gun：Electric spray ion source (ESI)；
Scan pattern：Positive ion mode；
Detection pattern：More reaction detection patterns (MRM), second order spectrum full scan.
It is further preferred that the testing conditions of step 4) are as follows：
Chromatographic column：HILIC posts, 100mm × 2.1mm, 1.7 μm；
Flow velocity：0.3mL/min；
Mobile phase：The volume ratio of acetonitrile/formic acid solution, acetonitrile and formic acid solution is 95：5, the volumetric concentration of formic acid solution
For 0.1%；
Sample size：5μL；
Column temperature：40℃；
Ion gun：Electric spray ion source；
Scan pattern：Positive ion mode；
Detection pattern：More reaction detection patterns, second order spectrum full scan, scanning range：30m/z~110m/z.
Preferably, step 4) condition of gradient elution is as follows：
| Chromatographic time/min | Aqueous formic acid (0.1%, v/v) | Acetonitrile/% |
| 0 | 5 | 95 |
| 2 | 5 | 95 |
| 4 | 15 | 85 |
| 7 | 5 | 95 |
Preferably, the testing conditions of more reaction detection patterns of step 4) are：
Second order spectrum full scan, scanning range 30m/z~110m/z.
Present disclosure is described in further detail below by way of specific embodiment.
Embodiment：
First, assay method
1st, reagent and material
Unless otherwise indicated, agents useful for same of the present invention is that analysis is pure, and water used meets one-level specified in GB/T 6682
Water.
1.1 reagent
1.1.1 glacial acetic acid (CH3COOH)。
1.1.2 acetonitrile (CH3CN)：Chromatographically pure.
1.2 preparation of reagents
1.2.1 acetum (0.05%)：Glacial acetic acid 0.5mL is measured, adds water to 1 000mL, is mixed.
1.3 reference material
1.3.1 thiourea dioxide (CH4N2O2S, CAS：1758-73-2)：Purity >=99%.
The preparation of 1.4 reference solutions
1.4.1 thiourea dioxide Standard Reserving Solution (1.0mg/mL)：Accurately weigh thiourea dioxide reference material 0.1g
(being accurate to 0.0001g), put in 100mL brown volumetric flasks, add acetum (0.05%, v/v) to dissolve and be settled to scale.In
4 DEG C of preservations, prepared on the day of use.
1.4.2 thiourea dioxide standard series working solution：Thiourea dioxide Standard Reserving Solution is diluted to step by step with acetonitrile
1.0 the μ g/mL of μ g/mL~100 standard series working solution.Face used time preparation, determined in 4 hours.
2nd, instrument and equipment
2.1 high performance liquid chromatographs, band PDAD.
2.2 assay balance：Sensibility reciprocal is 0.0001g.
2.3 ultrasonic cleaner.
3rd, analytical procedure
It is prepared by 3.1 samples
After sample is well mixed, it should be immediately available for detecting.
The preparation of 3.2 sample solutions
About 0.1g samples are weighed, are accurate to 0.0001g, are put in 100mL volumetric flasks, add acetum (0.05%, v/v) molten
Solve simultaneously constant volume, ice-water bath ultrasonic extraction 10min.Stood after being shaken to mixed, accurate Aspirate supernatant 1mL, put in 10mL volumetric flasks, add second
Nitrile is settled to scale.Through 0.45 μm of filtering with microporous membrane, subsequent filtrate is taken, is suitably diluted to according to actual concentrations in the range of linearity,
It is standby, determined in 4 hours.
3.3 instrument reference conditions
3.3.1 chromatographic column：Poroshell 120HILIC (150mm × 4.6mm, 2.7 μm).
3.3.2 flow velocity：1.0mL/min.
3.3.3 mobile phase：The volume ratio of acetonitrile/water, wherein acetonitrile and water is 9：1；
3.3.4 column temperature：30℃.
3.3.5 sample size：10μL.
3.3.6 PDAD wave-length coverage：190nm~600nm, or UV-detector Detection wavelength：
284nm。
3.3.7 gradient elution table is as follows.
| Time (min) | Water (%) | Acetonitrile (%) |
| 0 | 5 | 95 |
| 3 | 35 | 65 |
| 5.5 | 35 | 65 |
| 8 | 5 | 95 |
| 12 | 5 | 95 |
3.4 qualitative analysis
Sample solution and thiourea dioxide standard series working solution are injected separately into liquid chromatograph, when foundation retains
Between and line spectrum uniformity carry out qualitative recognition method, according to the retention time of thiourea dioxide reference material and in linear light
Spectrum, determine the chromatographic peak and spectrum peak of thiourea dioxide in sample.The liquid chromatogram of 20 μ g/mL thiourea dioxide reference materials
See accompanying drawing 1.
3.5 quantitative analysis
Sample solution and thiourea dioxide standard series working solution are injected separately into liquid chromatograph, measure is corresponding
Peak area, using the concentration of standard working solution as abscissa, using the peak area of chromatographic peak as ordinate, draw standard curve.According to
Standard curve obtains the sulfur dioxide urea concentration in sample solution.
4th, the statement of analysis result
The mass fraction X of thiourea dioxide content in sample, calculated by formula (1)：
In formula：
X --- the content of thiourea dioxide in sample, unit are gram every 100 grams (%)；
C --- the mass concentration of thiourea dioxide in sample solution, unit are micrograms per millilitre (μ g/mL)；
V --- sample dilutes cumulative volume, and unit is milliliter (mL)；
M --- sample mass, unit are gram (g).
Result of the test is defined by the arithmetic mean of instantaneous value of parallel determinations.The survey independent twice obtained under the conditions of repeatability
The absolute difference for determining result is not more than the 3% of arithmetic mean of instantaneous value.
The assay method of the present invention, when sample weighting amount is 0.1g, and extension rate is 1000, detection is limited to 1.0%, quantitative limit
For 3.0%.
5th, positive confirmatory analysis
Weigh and wait to confirm doubtful positive 0.1g (being accurate to 0.001g) in 100mL volumetric flasks, with 0.05% acetic acid
Water dissolves and is settled to scale.Precision measures 0.01mL in 10mL volumetric flasks, with 0.05% acetic acid water constant volume, is made into middle deposit
Liquid.Precision measures middle storing solution 1mL in 10mL volumetric flasks, with acetonitrile constant volume.After prepare liquid filtering with microporous membrane, machine is treated
Analysis.
Chromatographic column：HILIC posts, 100mm × 2.1mm, 1.7 μm；
Flow velocity：0.3mL/min；
Mobile phase：Acetonitrile/formic acid water (0.1%, v/v) solution, volume ratio 95：5；
Sample size：5μL；
Column temperature：40℃；
Condition of gradient elution is as follows：
| Chromatographic time/min | Aqueous formic acid (0.1%, v/v) | Acetonitrile/% |
| 0 | 5 | 95 |
| 2 | 5 | 95 |
| 4 | 15 | 85 |
| 7 | 5 | 95 |
Detection mode：The condition of multiple-reaction monitoring is as follows：
Second order spectrum full scan, scanning range 30m/z~110m/z.
2nd, apply
Using the present invention collected to certain illegal food processing producer two kinds of method without mark food bleaching agent A with
B, bleaching agent C (mark compositions are bought in market：Anhydrous sodium sulfite, sodium pyrosulfite), totally three parts of samples are detected.
Experimentation is as follows：
1st, sample pre-treatments：
Sample 0.1g (being accurate to 0.0001g) is weighed in 100mL volumetric flasks, is dissolved and is settled to 0.05% acetic acid water
Scale.Precision measures 1mL in 10mL volumetric flasks, with acetonitrile constant volume.After prepare liquid filtering with microporous membrane, treat that machine is analyzed.
The extension rate of test sample is 1000.
2nd, positive confirmation
Weigh and wait to confirm doubtful positive 0.1g (being accurate to 0.001g) in 100mL volumetric flasks, with 0.05% acetic acid
Water dissolves and is settled to scale.Precision measures 0.01mL in 10mL volumetric flasks, with 0.05% acetic acid water constant volume, is made into middle deposit
Liquid.Precision measures middle storing solution 1mL in 10mL volumetric flasks, with acetonitrile constant volume.After prepare liquid filtering with microporous membrane, machine is treated
Analysis.
As a result：
1st, spectrogram check analysis result is as follows：
By bleaching agent A DAD Fig. 3 compared with DAD Fig. 2 of thiourea dioxide reference material, and bleaching agent B DAD
For Fig. 4 compared with Fig. 2, its DAD figures are all consistent.Prove that bleaching agent A and bleaching agent B has detected thiourea dioxide.
2nd, MRM figures and the two level check analysis result that traces designs entirely are as follows：
By bleaching agent A MRM Fig. 7 compared with MRM Fig. 5 of thiourea dioxide reference material, both abundance of ions ratios
Unanimously.Compared with the full tracing 6 of the two level of thiourea dioxide reference material, both are also consistent for tracing 8 entirely for bleaching agent A two level.Institute
To demonstrate bleaching agent A and detect thiourea dioxide.
By bleaching agent B MRM Fig. 9 compared with MRM Fig. 5 of thiourea dioxide reference material, both abundance of ions ratios
Unanimously.Compared with the full tracing 6 of the two level of thiourea dioxide reference material, both are also consistent for tracing 10 entirely for bleaching agent B two level.Institute
To demonstrate bleaching agent B and detect thiourea dioxide.
According to testing result, bleaching agent C does not detect thiourea dioxide.
Claims (6)
- A kind of 1. assay method of thiourea dioxide in food additives, it is characterised in that：Comprise the following steps：1) extract：0.1g food additives are weighed, acetum dissolving is added, ice-water bath ultrasonic extraction, is settled to 100mL；2) sample solution is prepared：A, stand step 1) and obtain solution, take supernatant 1mL, 10mL is settled to acetonitrile, through 0.45 μm of membrane filtration, gained continues Filtrate is sample solution a；B, stand step 1) and obtain solution, take 0.01mL, 10mL is settled to acetum, be made into middle storing solution；Take centre Storing solution 1mL, 10mL is settled to acetonitrile, through 0.45 μm of membrane filtration, gained subsequent filtrate is sample solution b；3) detect：Sample solution a is detected using high performance liquid chromatography；4) confirm：Positive confirmation is carried out to sample solution b using tablets by HPLC-MS.
- 2. the assay method of thiourea dioxide in a kind of food additives according to claim 1, it is characterised in that：Acetic acid The volumetric concentration of solution is 0.05%.
- 3. the assay method of thiourea dioxide in a kind of food additives according to claim 1, it is characterised in that：Step 1) in, the time of ultrasonic extraction is 8~12min.
- 4. the assay method of thiourea dioxide in a kind of food additives according to claim 1, it is characterised in that：Efficiently Instrument used in liquid chromatography is the high performance liquid chromatograph with PDAD or UV-detector.
- 5. the assay method of thiourea dioxide in a kind of food additives according to claim 1, it is characterised in that：Step 3) testing conditions are as follows：Chromatographic column：HILIC posts, 150mm × 4.6mm, 2.7 μm；Flow velocity：0.8~1.2mL/min；Sample size：10μL；Column temperature：28~32 DEG C；PDAD wave-length coverage：190~600nm；Or UV-detector Detection wavelength：284nm.
- 6. the assay method of thiourea dioxide in a kind of food additives according to claim 1, it is characterised in that：Step 4) testing conditions are as follows：Chromatographic column：HILIC posts, 100mm × 2.1mm, 1.7 μm；Flow velocity：0.2~0.3mL/min；Sample size：5μL；Column temperature：38~42 DEG C；Ion gun：Electric spray ion source；Scan pattern：Positive ion mode；Detection pattern：More reaction detection patterns, second order spectrum full scan.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108828113A (en) * | 2018-06-06 | 2018-11-16 | 广州市食品检验所（广州市酒类检测中心） | A method of measurement thiourea dioxide in food content |
| CN111999130A (en) * | 2020-08-31 | 2020-11-27 | 重庆惠能标普科技有限公司 | Anti-oxidation absorption liquid for collecting sulfur dioxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108828113A (en) * | 2018-06-06 | 2018-11-16 | 广州市食品检验所（广州市酒类检测中心） | A method of measurement thiourea dioxide in food content |
| CN111999130A (en) * | 2020-08-31 | 2020-11-27 | 重庆惠能标普科技有限公司 | Anti-oxidation absorption liquid for collecting sulfur dioxide and preparation method thereof |
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Application publication date: 20171212 |