CN205484229U - A solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey - Google Patents
A solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey Download PDFInfo
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- CN205484229U CN205484229U CN201521119939.6U CN201521119939U CN205484229U CN 205484229 U CN205484229 U CN 205484229U CN 201521119939 U CN201521119939 U CN 201521119939U CN 205484229 U CN205484229 U CN 205484229U
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- phase extraction
- vanillin
- solid
- ethyl vanillin
- molecular engram
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Abstract
The utility model discloses a set gradually three circular polyethylene sieves from last under to in a solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey, the cylinder of this solid -phase extraction post, separated into two layers of packing cavity space with tubulose cylinder inner chamber, be provided with vanillic aldehyde molecular engram solid -phase extraction packing layer in the upper space, be provided with ethyl vanillin molecular engram solid -phase extraction packing layer in the lower floor space, tubulose cylinder bottom along radially narrowing and putting the formation drain pipe at central point, this solid -phase extraction post has simple structure, convenient to use and characteristics with low costs can shorten the sample pretreatment time effectively, can be applied to fill a prescription in the food survey of vanillic aldehyde and ethyl vanillin of infant betterly.
Description
Technical field:
This utility model belongs to analytical chemistry facility, is specifically related to a kind of special solid-phase extraction column that vanillin and ethyl vanillin measure in dispensed food for baby.
Background technology:
Vanillin (Vanillin), have another name called vanillin, formal name used at school Vanillin, ethyl vanillin, formal name used at school vanirom, can find in the seed of vanilla, can also synthetic, both of which is odor additive important in food, it is widely used in various perfumery food, the standard GB/T 2760 " national food safety standard food additive uses standard " of China allows to use vanillin in bigger infants and young's formula food, ethyl vanillin, and be used for limitation and dictate, but dispensed food for baby must not add any food spice in 0 to 6 month.In addition, the Committee of Experts of European Union is through experimental studies have found that for many years, heavy dose of vanillin that uses has bigger harm to human body, excessively take in and may result in headache, Nausea and vomiting, dyspnea, even damage Liver and kidney etc., therefore, it is quite necessary to the service condition of vanillin in dispensed food for baby and ethyl vanillin is monitored.
nullAt present，Vanillin in food and ethyl vanillin only finite quantity are specified by national standard，And there is no the standard of detection method，And generally the detection method of vanillin in food and ethyl vanillin is had gas chromatogram、Liquid chromatograph、Gas chromatography mass spectrometry、The method such as LC-MS or capillary electrophoresis，Pre-treatment means have liquid-liquid extraction or Solid-Phase Extraction etc.，Liquid-liquid extraction is suitable for fluid sample or vanillin and the higher sample of ethyl vanillin content，For the method adding a small amount of vanillin in dispensed food for baby and ethyl vanillin is more suitable for using Solid-Phase Extraction，And it is currently used for extraction and cleaning vanillin and ethyl vanillin is used a solid-phase extraction column，The most universal C18 post or ion exchange column，These solid-phase extraction columns do not possess specificity to the extraction of vanillin and ethyl vanillin，Therefore the response rate is unstable，Simultaneously because the sample substrate of dispensed food for baby is complicated，Use this do not have specific solid phase extraction purify，Partial impurities also can be extracted，Clean-up effect is the best，Therefore，Prepare high specificity、Vanillin in dispensed food for baby and the special solid-phase extraction column of ethyl vanillin mensuration that stability is high are particularly significant.
Utility model content:
For the deficiencies in the prior art; the purpose of this utility model is to provide a kind of solid-phase extraction column that vanillin and ethyl vanillin measure in infant food; this solid-phase extraction column uses a small amount of solvent just to can reach the effect of sample purification; and simultaneously efficiently concentrating vanillin and ethyl vanillin; there is simplification sample handling procedure, save sample processing time the advantage protecting environment.
Realize this utility model above-mentioned purpose to be adopted the technical scheme that:
A kind of solid-phase extraction column that vanillin and ethyl vanillin measure in infant food, there is the tubular cylinder that a polypropylene material is made, described tubular cylinder upper end open, feature is, described tubular cylinder inner chamber is disposed with three pieces of round polyethylene sieve plates from top to bottom, tubular cylinder inner chamber is separated into two layers of packing cavity space, in upper sheaf space, is provided with vanillin molecular engram solid phase extraction filler layer, in lower layer space, be provided with ethyl vanillin molecular engram solid phase extraction stuffing layer；Radially narrow bottom tubular cylinder and form drain pipe in center.
Preferably, the aperture of described polyethylene sieve plate is 20 μm.
Preferably, a length of 66mm of described tubular cylinder, internal diameter is 12.7mm.
Preferably, the vanillin molecular engram solid phase extraction filler layer arranged in described upper sheaf space is 200mg, and the ethyl vanillin molecular engram solid phase extraction stuffing layer arranged in lower layer space is 200mg.
The beneficial effects of the utility model are: be separated into 2 layers with 3 sieve plates in tubular cylinder, load 2 kinds of fillers, once cross post and just can reach the effect of Sync enrichment vanillin and ethyl vanillin, extraction effect is good, compare with ion exchange column with conventional C18 post, higher to the extraction specificity of object, clean-up effect is more preferable, and the response rate is stable.Vanillin and the feature of ethyl vanillin pre-treating method during this solid-phase extraction column is primarily directed to dispensed food for baby simultaneously and design, optimize solid-phase extraction column cavity volume, ratio between vanillin and ethyl vanillin molecular engram solid phase extraction stuffing, in the case of ensureing the good method response rate, add less amount of solid phase extraction filler, reach to purify and the purpose of enrichment, reduce cost, and reduce the error brought by experimenter's technical capability difference, improve vanillin and the accuracy of ethyl vanillin quantitative analysis.
Accompanying drawing illustrates:
Fig. 1 is structural representation of the present utility model.
Wherein label: 1 is cylinder；2 is vanillin molecular engram solid phase extraction filler；3 is ethyl vanillin molecular engram solid phase extraction stuffing；4 is polyethylene sieve plate.
Detailed description of the invention:
Below in conjunction with the accompanying drawing in this utility model embodiment, the technical scheme in this utility model embodiment is clearly and completely described, it is clear that described embodiment is only a part of embodiment of this utility model rather than whole embodiments.
Embodiment 1:
Seeing Fig. 1, Solid-Phase Extraction cylinder 1 of the present utility model all uses polyacrylic material to make column jecket shape, and the internal diameter of column jecket is 12.7mm, a length of 66mm of column jecket, and the aperture of polyethylene sieve plate 4 is 20 μm.First bottom empty tubular cylinder, load a piece of polyethylene sieve plate 4, it is then charged into the ethyl vanillin molecular engram solid phase extraction stuffing 3 of 200mg, reinstall a piece of polyethylene sieve plate 4 to be compacted by filler 3, it is then charged into the vanillin molecular engram solid phase extraction filler 2 of 200mg, finally loading a piece of polyethylene sieve plate 4 and be compacted filler 2, solid-phase extraction column i.e. loads complete.
Vanillin molecular engram solid phase extraction filler 2 and ethyl vanillin molecular engram solid phase extraction stuffing 3 can be by commercially available acquisitions.
Vanillin molecular engram solid phase extraction filler 2 can also be prepared by the following:
The preparation of vanillin molecular engram solid phase extraction filler:
Weigh the vanillin of 152mg, put in 100mL round-bottomed flask, add the 2-methacrylic acid of 0.5g and the 2-methyl-2-acrylic acid-1 of 3g, 2-glycol ester, the ratio adding 40mL is in 1:10 water/alcohol mixed solvent, fully mixes dissolving, adds the azodiisobutyronitrile of 40mg.It is filled with nitrogen 10min, mixed solution is oscillating reactions 24 hours under 60 DEG C of water bath condition, taking-up bulk polymer grinds, cross 200 ~ 300 mesh sieves, the polymer beads fast qualitative filter paper of collection is wrapped, puts in Soxhlet extractor, the ratio of 500mL is that 1:9 acetic acid/methanol mixed solvent extracts 24 hours, extracting 24 hours with 500mL methanol, remove unnecessary vanillin, 60 DEG C of vacuum drying obtain vanillin molecular engram solid phase extraction filler.
Ethyl vanillin molecular engram solid phase extraction stuffing 3 can also be prepared by the following:
The preparation of ethyl vanillin molecular engram solid phase extraction stuffing
Weigh the ethyl vanillin of 166mg, put in 100mL round-bottomed flask, add the 2-methacrylic acid of 0.5g and the 2-methyl-2-acrylic acid-1 of 3g, 2-glycol ester, the ratio adding 40mL is in 1:10 water/alcohol mixed solvent, fully mixes dissolving, adds the azodiisobutyronitrile of 40mg.It is filled with nitrogen 10min, mixed solution is oscillating reactions 24 hours under 60 DEG C of water bath condition, taking-up bulk polymer grinds, cross 200 ~ 300 mesh sieves, the polymer beads fast qualitative filter paper of collection is wrapped, puts in Soxhlet extractor, the ratio of 500mL is that 1:9 acetic acid/methanol mixed solvent extracts 24 hours, extracting 24 hours with 500mL methanol, remove unnecessary ethyl vanillin, 60 DEG C of vacuum drying obtain ethyl vanillin molecular engram solid phase extraction stuffing.
Embodiment 2:
Weigh baby formula milk powder sample 1g, put in 50mL test tube, add the water dissolution of 5mL, it is settled to 50mL again with ethanol, vibration mixing, use fast qualitative filter paper filtering, collect filtrate, then draw, the filtrate of 10mL is added on the solid-phase extraction column that embodiment 1 obtains, remove impurity with 5mL ultra-pure water drip washing again, then with 10mL methanol solution eluting, collect eluent in test tube, ambient temperature using nitrogen is slowly blown near dry, by methanol constant volume to 1mL, cross 0.45 μm organic facies filter membrane, for gas chromatograph-mass spectrometer analysis.
The foregoing is only preferred embodiment of the present utility model; not in order to limit this utility model; all within spirit of the present utility model and principle, any modification, equivalent substitution and improvement etc. made, within should be included in protection domain of the present utility model.
Claims (2)
1. the solid-phase extraction column that vanillin and ethyl vanillin measure in infant food, there is the tubular cylinder that a polypropylene material is made, described tubular cylinder upper end open, it is characterized in that, described tubular cylinder inner chamber is disposed with three pieces of round polyethylene sieve plates from top to bottom, tubular cylinder inner chamber is separated into two layers of packing cavity space, in upper sheaf space, is provided with vanillin molecular engram solid phase extraction filler layer, in lower layer space, be provided with ethyl vanillin molecular engram solid phase extraction stuffing layer；Radially narrow bottom tubular cylinder and form drain pipe in center；
The a length of 66mm of described tubular cylinder, internal diameter is 12.7mm；The vanillin molecular engram solid phase extraction filler layer arranged in described upper sheaf space is 200mg, and the ethyl vanillin molecular engram solid phase extraction stuffing layer arranged in lower layer space is 200mg.
2. the solid-phase extraction column that vanillin and ethyl vanillin measure in infant food as claimed in claim 1, it is characterised in that: the aperture of described polyethylene sieve plate is 20 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521119939.6U CN205484229U (en) | 2015-12-30 | 2015-12-30 | A solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521119939.6U CN205484229U (en) | 2015-12-30 | 2015-12-30 | A solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey |
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| Publication Number | Publication Date |
|---|---|
| CN205484229U true CN205484229U (en) | 2016-08-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201521119939.6U Expired - Fee Related CN205484229U (en) | 2015-12-30 | 2015-12-30 | A solid -phase extraction post that is arranged in infant food vanillic aldehyde and ethyl vanillin to survey |
Country Status (1)
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| CN (1) | CN205484229U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724623A (en) * | 2019-09-10 | 2020-01-24 | 深圳市百迈生命科学有限公司 | 1536 well solid phase synthesis and extraction plate |
| CN113203817A (en) * | 2021-04-16 | 2021-08-03 | 云南中烟工业有限责任公司 | Method for rapidly detecting ethyl vanillin beta-D-glucoside in cigarette paper |
-
2015
- 2015-12-30 CN CN201521119939.6U patent/CN205484229U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724623A (en) * | 2019-09-10 | 2020-01-24 | 深圳市百迈生命科学有限公司 | 1536 well solid phase synthesis and extraction plate |
| CN113203817A (en) * | 2021-04-16 | 2021-08-03 | 云南中烟工业有限责任公司 | Method for rapidly detecting ethyl vanillin beta-D-glucoside in cigarette paper |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160817 Termination date: 20181230 |