CN103163129A - Detection method for content of polyhexamethylene guanidine - Google Patents
Detection method for content of polyhexamethylene guanidine Download PDFInfo
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- CN103163129A CN103163129A CN2013100907245A CN201310090724A CN103163129A CN 103163129 A CN103163129 A CN 103163129A CN 2013100907245 A CN2013100907245 A CN 2013100907245A CN 201310090724 A CN201310090724 A CN 201310090724A CN 103163129 A CN103163129 A CN 103163129A
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- 238000001514 detection method Methods 0.000 title claims abstract description 39
- -1 polyhexamethylene guanidine Polymers 0.000 title abstract description 8
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims abstract description 41
- JKMHFZQWWAIEOD-UHFFFAOYSA-N 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid Chemical compound OCC[NH+]1CCN(CCS([O-])(=O)=O)CC1 JKMHFZQWWAIEOD-UHFFFAOYSA-N 0.000 claims abstract description 32
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims abstract description 21
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229940089468 hydroxyethylpiperazine ethane sulfonic acid Drugs 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 229920002413 Polyhexanide Polymers 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 33
- 239000012086 standard solution Substances 0.000 claims description 29
- 238000012360 testing method Methods 0.000 claims description 25
- 239000007995 HEPES buffer Substances 0.000 claims description 23
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 21
- 229940005654 nitrite ion Drugs 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000013016 damping Methods 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 14
- 239000010931 gold Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 230000031700 light absorption Effects 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- 230000000007 visual effect Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002798 spectrophotometry method Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000010561 standard procedure Methods 0.000 abstract description 3
- 229940123208 Biguanide Drugs 0.000 description 7
- 150000004283 biguanides Chemical class 0.000 description 7
- 230000001954 sterilising effect Effects 0.000 description 5
- 238000004659 sterilization and disinfection Methods 0.000 description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000012800 visualization Methods 0.000 description 4
- VAZJLPXFVQHDFB-UHFFFAOYSA-N 1-(diaminomethylidene)-2-hexylguanidine Polymers CCCCCCN=C(N)N=C(N)N VAZJLPXFVQHDFB-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000012417 linear regression Methods 0.000 description 3
- 229920001213 Polysorbate 20 Polymers 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000003093 cationic surfactant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002357 guanidines Chemical class 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 2
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 229940098773 bovine serum albumin Drugs 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- SAGIGHPRUJPLKX-UHFFFAOYSA-N n'-[6-[(n'-methylcarbamimidoyl)amino]hexyl]ethanimidamide Chemical compound CN=C(N)NCCCCCCN=C(C)N SAGIGHPRUJPLKX-UHFFFAOYSA-N 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000004366 reverse phase liquid chromatography Methods 0.000 description 1
- 239000012898 sample dilution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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Abstract
The invention relates to a detection method for content of effective element of guanidine and particularly relates to a detection method for the content of polyhexamethylene guanidine. The preparation method comprises the steps of: utilizing negatively charged nanogold solution with the grain diameter of 13-35 nm as an indicator, utilizing a spectrophotometer or a colorimetric card as a detection device, and utilizing HEPES (hydroxyethyl piperazine ethanesulfonic acid) solution as buffer liquid, thus detecting the content of the polyhexamethylene guanidine. The detection method for the content of the polyhexamethylene guanidine has the advantages that (1) the sensitivity of the detection method is high, and the anti-interference performance is strong; and (2) the concentration of the polyhexamethylene guanidine in a to-be-measured sample can be visually detected on site by utilizing the colorimetric card but cannot be detected by utilizing a national standard method.
Description
Technical field
The present invention relates to a kind of detection method of guanidine active constituent content, specifically, relate to a kind of detection method of polyhexamethylene guanide content.
Background technology
Polyhexamethylene guanide is a kind of macromolecule cation polymer, common are polyhexamethylene list guanidinesalt hydrochlorate (PHMG-HCl) and hexamethylene (PHMB-HCl), and is all soluble in water.The colourless odorlessness of its aqueous solution has extremely strong kill bacteria ability and long-term bacteriostasis, is commonly used for the sterilization of external application medicine equipment and skin, wound, the public health articles for use such as air, wall, ground, lavatory and the dustbin sterilization in ward.
As environment-friendly type macromolecule polymkeric substance disinfection sanitizer, polyhexamethylene guanide has the sterilization wide spectrum, effective concentration is low, speed of action is fast, stable in properties, soluble in water, can use at normal temperatures, for a long time antibacterial, have no side effect, non-corrosiveness, colourless, odorless, nontoxic, do not fire, not quick-fried, use safety, the advantages such as convenient transportation.It can be widely used in food-processing industry, potable water and swimming sterilizing, commodity sterilization, building materials industry, textile industry, paper-making industry, wood-processing industry, rubber industry, oil exploitation, the agricultural aquatic products is herded the industries such as secondary fishing.
The detection method of traditional polyhexamethylene guanide mainly contains following several:
1, reversed phase liquid chromatography: the method complex steps, equipment needed thereby are expensive, the testing result accuracy is not high.
2, the assay method (GB26367-2010) of national standard detection method-poly hexamethylene biguanide content: this method adopts spectrophotometer to detect, do not need expensive device, more for convenience, but this method colour developing is not obvious, be difficult to naked eyes and differentiate, can't visualization of presence detect testing sample.
3, colloid titration method: the method complex operation, easily be disturbed, sensitivity is not high yet.
Summary of the invention
For solving the problems of the technologies described above, the present invention proposes a kind of step simple, highly sensitive, disturb little and need not expensive checkout equipment, method that can on-the-spot visual detection polyhexamethylene guanide content.
Technical scheme of the present invention is: a kind of detection method of polyhexamethylene guanide content, and adopt the nano-Au solution of electronegative, particle diameter 13-35nm as indicator, adopt spectrophotometer or colorimetric card to detect polyhexamethylene guanide content as checkout equipment.
The detection method of described polyhexamethylene guanide content adopts the HEPES(hydroxyethyl piperazine ethanesulfonic acid) solution is as damping fluid.
The concrete steps of the detection method of described polyhexamethylene guanide content are as follows:
1, prepare standard solution and reagent: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution.
2, preparation nitrite ion and dilution:
1) nano-Au solution of anamorphic zone negative charge, its maximum absorption wavelength 520 ± 5nm, particle diameter 13-35nm;
The compound method of nano-Au solution is: add 2ml in 93ml water, after 1% chlorauric acid solution ebuillition of heated, then add 5ml, 1% sodium citrate solution continues heating 20 minutes, is cooled to room temperature standby.
2) secure ph is between 6-8, the HEPES(hydroxyethyl piperazine ethanesulfonic acid of 1mol/L) solution is as damping fluid;
The compound method of HEPES damping fluid is: take 260.39 gram HEPES and add the distilled water dissolving, regulate pH value 6 to 8, be settled to 1L and get final product.
3) nano-Au solution and the HEPES damping fluid that preparation nitrite ion: with step 1) and 2) make mix, and HEPES solution ultimate density is less than 100mmol/L.
4) the HEPES damping fluid that prepared and diluted liquid: with step 2) makes mixes with distilled water, and HEPES solution ultimate density is less than 100mmol/L.
3, adopt spectrophotometer as checkout equipment, by polyhexamethylene guanide concentration in drawing standard curve detection testing sample.Concrete steps are as follows:
(1) the poly-hexamethyl guanidine standard solution of preparation variable concentrations, at least three concentration;
(2) get poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, reacted 5 minutes;
(3) drawing standard curve: with the spectrophotometer measurement above-mentioned steps 3-(2) light absorption value between wavelength 600 to 700 nanometers of Plays solution, at least the detection of each concentration standard solution three times, average, take the polyhexamethylene guanide concentration of standard solution as horizontal ordinate, take the absorptivity of each concentration standard solution as ordinate, the drawing standard curve.
(4) get testing sample, add isopyknic nitrite ion, reacted 5 minutes, with the light absorption value of spectrophotometric determination testing sample between wavelength 600 to 700 nanometers, at step 3-(3) check in corresponding concentration value on the typical curve drawn.
A, making colorimetric card;
B, get testing sample, add isopyknic nitrite ion, colour generation;
C, with standard color comparison card visual colorimetric determination from top to bottom, the color corresponding concentration close with the standard color comparison card tone is namely the content of polyhexamethylene guanide in testing sample.
In above-mentioned steps a, the method for making of colorimetric card is: preparation 0.05ppm is to the poly-hexamethyl guanidine standard solution of 0.5ppm, and at least three concentration are got a standard solution, add isopyknic sample and nitrite ion, mixing was taken pictures with digital camera after 5 minutes, after image is processed, colour print.
Principle of the present invention is: under neutrallty condition, positively charged and the electronegative nm of gold of the guanidine radicals of poly-hexamethyl guanidine is passed through the static interaction, the Partial charge on the nm of gold has neutralized, make nm of gold assemble, and produce the distinguishable change color of corresponding naked eyes, the content of the light absorption value of its 600 to 700 nanometers and poly-hexamethyl guanidine is proportional, can use the spectrophotometer realization to the quantitative detection of polyhexamethylene guanide, can also use colorimetric card to carry out visual detection.
Beneficial effect of the present invention is:
1, the present invention is good to assay method (GB26367-2010) correlativity of polyhexamethylene guanide sample tests value and national standard detection method-poly hexamethylene biguanide content, and good in concentration 0.05-0.5ppm scope internal linear, detection is limited to 0.05ppm, higher than the sensitivity of bibliographical information at present.
2, the present invention can both measure poly-six subunit list guanidines and poly-six subunit biguanides, and the salt ion of common cationic surfactant, anionic surfactant, non-ionic surfactant, organism and high concentration is interference measurement not, strong interference immunity.
3, the present invention can also adopt the polyhexamethylene guanide concentration in colorimetric card visualization of presence detection testing sample, and National Standard Method can't detect.
Description of drawings
Fig. 1 is the canonical plotting of drawing in the present invention;
Fig. 2 is the present invention and national standard detection method correlativity comparison diagram;
Fig. 3 be the present invention to the test experience figure of different analytes, the ordinate in figure represents the light absorption value at 670nm place;
Wherein, in Fig. 3, the sequence number of horizontal ordinate is described as follows:
1, poly-six subunit biguanides (PHMB) standard items of 5ppm; 2, poly-six subunit list guanidine (PHMG) standard items of 5ppm; 3,5ppm cetyl trimethyl ammonium bromide (CTAB); 4,0.1% bovine serum albumin(BSA); 5,0.05% lauryl sodium sulfate; 6,0.05%Tween20; 7,145mmol/L NaCl;
Fig. 4 is that the present invention adopts the colorimetric card visualization of presence to detect testing sample figure,
Wherein, Fig. 4 the first row is to adopt colorimetric block-regulations provided by the invention to detect the pattern of poly-six subunit biguanides concentration, the second row is to adopt the colorimetric block-regulations that National Standard Method provides to detect the pattern that gathers six subunit biguanides concentration, and in figure, numeral is the concentration of poly-six subunit biguanides in solution, unit: ppm.
Embodiment
Illustrate the present invention below in conjunction with drawings and Examples.
Embodiment 1:
A kind of detection method of polyhexamethylene guanide content, concrete steps are as follows:
1, prepare standard solution and reagent: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution.
2, preparation nitrite ion and dilution:
1) nano-Au solution of anamorphic zone negative charge:
Add 2ml, 1% chlorauric acid solution ebuillition of heated in 93ml water after, then add 5ml, 1% sodium citrate solution, continue heating 20 minutes, be cooled to room temperature standby.Synthetic nano-Au solution, electronegative, maximum absorption wavelength is in 520 ± 5 nanometers, and particle diameter is between the 13-35 nanometer;
2) secure ph is between 6-8, the HEPES(hydroxyethyl piperazine ethanesulfonic acid of 1mol/L) solution is as damping fluid;
The compound method of HEPES damping fluid is: take 260.39 gram HEPES and add the distilled water dissolving, regulate pH value 6 to 8, be settled to 1L and get final product.
3) nano-Au solution and the HEPES damping fluid that preparation nitrite ion: with step 1) and 2) make mix by the 20:1 volume ratio, and HEPES solution ultimate density is 100mmol/L.
4) the HEPES damping fluid that prepared and diluted liquid: with step 2) makes mixes by the 1:20 volume ratio with distilled water, and HEPES solution ultimate density is 100mmol/L.
3, adopt spectrophotometer as checkout equipment, by polyhexamethylene guanide concentration in drawing standard curve detection testing sample.Concrete steps are as follows:
(1) compound concentration is the poly-hexamethyl guanidine standard solution of series of 0.05-0.5ppm, makes its concentration be respectively 0ppm, 0.03125ppm, 0.0625ppm, 0.125ppm, 0.25ppm, 0.5ppm;
(2) get poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, reacted 5 minutes;
(3) drawing standard curve: with spectrophotometer measurement above-mentioned steps 3-(2) Plays solution is at the light absorption value of wavelength 670 nanometers, each concentration standard solution detects three times at least, average, take the polyhexamethylene guanide concentration of standard solution as horizontal ordinate, take the absorptivity of each concentration standard solution as ordinate, the drawing standard curve, and do linear regression, see Fig. 1, the typical curve equation is: y=0.2584x-0.0152(R
2=0.9999, n=6).
(4) get testing sample, add isopyknic nitrite ion, reacted 5 minutes, with the light absorption value of spectrophotometer measurement wavelength in 670 nanometers.Check in corresponding concentration value on the typical curve that step (3) is drawn.
(5) can be drawn by equation of linear regression, poly-hexamethyl guanidine is linear good in the 0-0.5ppm scope, detects and is limited to 0.05ppm, higher than the sensitivity of bibliographical information at present.
Embodiment 2:
The present invention and national standard detection method correlativity are relatively
(1) compound concentration is the poly-hexamethyl guanidine standard solution of series of 0.05-0.5ppm, makes its concentration be respectively 0ppm, 0.03125ppm, 0.0625ppm, 0.125ppm, 0.25ppm, 0.5ppm;
(2) get a poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, reacted 5 minutes;
(3) drawing standard curve: with the light absorption value of spectrophotometer measurement above-mentioned steps (2) Plays solution wavelength in 670 nanometers, each sample detects three times at least, average, take the polyhexamethylene guanide concentration of standard solution as horizontal ordinate, take each absorption of sample rate as ordinate, the drawing standard curve, and do linear regression, the typical curve equation is: y=0.2584x-0.0152(R
2=0.9999, n=6).
(4) get 1000 times of 20 parts of different Sample Dilutions after, add respectively sample and nitrite ion after isopyknic dilution, reacted 5 minutes, with the light absorption value of spectrophotometer measurement wavelength in 670 nanometers.Check in corresponding concentration value on the typical curve that step (3) is drawn, and result be multiply by 1000 times, be the concentration of sample.
(5) press the concentration value of 20 parts of different samples in assay method (GB26367-2010) determination step (4) of national standard detection method-poly hexamethylene biguanide content, and carried out correlativity relatively, result shows, significant correlation between the two, dependent equation is y=1.076x-1.0883(R=0.99), see Fig. 2, meet national standard and the actual requirement of using.
Embodiment 3:
Test experience to different analytes
poly-six subunit biguanides (PHMB) standard items with 5ppm, poly-six subunit list guanidine (PHMG) standard items of 5ppm, 5ppm cetyl trimethyl ammonium bromide (CTAB), 0.1%BSA, 0.05%SDS, 0.05%Tween20, 145mmol/L NaCl is as analyte, sample compares by volume with nitrite ion, and 1:9 adds, after mixing, sample measurement is at the light absorption value of 670nm wavelength after 5 minutes, as shown in Figure 3, result shows this kit no matter be poly-six subunit list guanidines, or poly-six subunit biguanides can both be measured, and to common cationic surfactant, anionic surfactant, non-ionic surfactant, the salt ion of organism and high concentration all has certain antijamming capability, can be used for the detection of the poly-hexamethyl guanidine of water body.
Embodiment 4:
Colorimetric card making and visual colorimetry detect the comparative experiments of testing sample
The poly-hexamethyl guanidine standard solution of preparation 0-5ppm, at least three concentration add equal-volume sample and nitrite ion in 96 orifice plates, and mixing was taken pictures with digital camera after 5 minutes, and colorimetric card is made in colour print after image is processed.Get the sample of six variable concentrations, ratio in 1:9 in 96 orifice plates adds sample and nitrite ion, mix, after 5 minutes with standard color comparison card visual colorimetric determination from top to bottom, the color corresponding concentration close with the standard color comparison card tone is namely the content of polyhexamethylene guanide in testing sample, its testing result and setting value are suitable, see Fig. 4, show that this law can bore hole differentiates the tone of the poly-hexamethyl guanidine of different concentration, can visualization of presence detect testing sample, and the GB rule is difficult to differentiate.
Claims (7)
1. the detection method of a polyhexamethylene guanide content, it is characterized in that, its nano-Au solution that adopts electronegative, particle diameter 13-35nm adopts spectrophotometer or colorimetric card as checkout equipment as indicator, adopt HEPES solution as damping fluid, detect polyhexamethylene guanide content.
2. the detection method of polyhexamethylene guanide content according to claim 1, is characterized in that, concrete steps are as follows:
1) prepare standard solution and reagent: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution;
2) preparation nitrite ion and dilution:
The nano-Au solution of a, anamorphic zone negative charge, its maximum absorption wavelength 520 ± 5nm, particle diameter 13-35nm;
B, secure ph between 6-8, the HEPES(hydroxyethyl piperazine ethanesulfonic acid of 1mol/L) solution is as damping fluid;
C, preparation nitrite ion: nano-Au solution and HEPES damping fluid that step a and b are made mix, and HEPES solution ultimate density is less than 100mmol/L;
D, prepared and diluted liquid: the HEPES damping fluid with step b makes, to mix with distilled water, HEPES solution ultimate density is less than 100mmol/L;
3) adopt spectrophotometer as checkout equipment, by polyhexamethylene guanide concentration in drawing standard curve detection testing sample.
3. the detection method of polyhexamethylene guanide content according to claim 2, is characterized in that, the concrete steps of described step 3) are as follows:
(1) the poly-hexamethyl guanidine standard solution of preparation variable concentrations, at least three concentration;
(2) get poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, reacted 5 minutes;
(3) drawing standard curve: with the spectrophotometer measurement above-mentioned steps 3-(2) light absorption value between wavelength 600 to 700 nanometers of Plays solution, at least the detection of each concentration standard solution three times, average, take the polyhexamethylene guanide concentration of standard solution as horizontal ordinate, take the absorptivity of each concentration standard solution as ordinate, the drawing standard curve;
(4) get testing sample, add isopyknic nitrite ion, reacted 5 minutes, with the light absorption value of spectrophotometric determination testing sample between wavelength 600 to 700 nanometers, at step 3-(3) check in corresponding concentration value on the typical curve drawn.
4. the detection method of polyhexamethylene guanide content according to claim 2, is characterized in that, described step 3) can also be: adopt the polyhexamethylene guanide concentration in colorimetric card detection testing sample, concrete steps are as follows:
(1) make colorimetric card;
(2) get testing sample, add isopyknic nitrite ion, colour generation;
(3) with standard color comparison card visual colorimetric determination from top to bottom, the color corresponding concentration close with the standard color comparison card tone is namely the content of polyhexamethylene guanide in testing sample.
5. the detection method of polyhexamethylene guanide content according to claim 4, it is characterized in that, in described step (1), the method for making of colorimetric card is: preparation 0.05ppm is to the poly-hexamethyl guanidine standard solution of 0.5ppm, at least three concentration are got a standard solution, add isopyknic sample and nitrite ion, mixing, take pictures with digital camera after 5 minutes, after image is processed, colour print.
6. the detection method of polyhexamethylene guanide content according to claim 2, it is characterized in that, described step 2) in-a, the compound method of nano-Au solution is: add 2ml in 93ml water, after 1% chlorauric acid solution ebuillition of heated, add again 5ml, 1% sodium citrate solution continues heating 20 minutes, is cooled to room temperature standby.
7. the detection method of polyhexamethylene guanide content according to claim 2, is characterized in that, described step 2)-b in the compound method of HEPES damping fluid be: take 260.39 gram HEPES and add the distilled water dissolving, regulate pH value 6 to 8, be settled to 1L and get final product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101503638B1 (en) | 2014-01-29 | 2015-03-17 | 영남대학교 산학협력단 | Detection method and kit of fatal sterilizer in household products |
| RU2557930C1 (en) * | 2014-06-04 | 2015-07-27 | Региональная общественная организация-Институт эколого-технологических проблем (РОО ИЭТП) | Method of quantitative determination of concentration of polyhexamethyleneguanidine hydrochloride in water solution |
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Cited By (2)
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| KR101503638B1 (en) | 2014-01-29 | 2015-03-17 | 영남대학교 산학협력단 | Detection method and kit of fatal sterilizer in household products |
| RU2557930C1 (en) * | 2014-06-04 | 2015-07-27 | Региональная общественная организация-Институт эколого-технологических проблем (РОО ИЭТП) | Method of quantitative determination of concentration of polyhexamethyleneguanidine hydrochloride in water solution |
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