CN103163129B - Detection method for content of polyhexamethylene guanidine sanitizer - Google Patents
Detection method for content of polyhexamethylene guanidine sanitizer Download PDFInfo
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- CN103163129B CN103163129B CN201310090724.5A CN201310090724A CN103163129B CN 103163129 B CN103163129 B CN 103163129B CN 201310090724 A CN201310090724 A CN 201310090724A CN 103163129 B CN103163129 B CN 103163129B
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- 238000001514 detection method Methods 0.000 title claims abstract description 38
- -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
- 229940089468 hydroxyethylpiperazine ethane sulfonic acid Drugs 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 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 229920002413 Polyhexanide Polymers 0.000 claims description 44
- 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
- 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
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000005259 measurement Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 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
- 238000004659 sterilization and disinfection Methods 0.000 claims description 6
- 230000000007 visual effect Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 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
- 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
- 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
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000010561 standard procedure Methods 0.000 abstract description 3
- 229960004198 guanidine Drugs 0.000 description 17
- 229940123208 Biguanide Drugs 0.000 description 7
- 150000004283 biguanides Chemical class 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
- 230000001954 sterilising effect Effects 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
- XNCOSPRUTUOJCJ-UHFFFAOYSA-N Biguanide Chemical compound NC(N)=NC(N)=N XNCOSPRUTUOJCJ-UHFFFAOYSA-N 0.000 description 2
- 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
- 238000004458 analytical method Methods 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
- 230000015572 biosynthetic process 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
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 244000144980 herd Species 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
- 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
- 230000007935 neutral effect Effects 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
- 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
- 239000000126 substance Substances 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
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 guanidine hydrochloride (PHMG-HCl) and hexamethylene (PHMB-HCl), 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 public health articles for use sterilizations such as external medical apparatus and skin, the sterilization of wound, the air in ward, wall, ground, lavatory and dustbin.
As environment-friendly type macromolecule polymkeric substance disinfection sanitizer, polyhexamethylene guanide has broad-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, 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, agricultural aquatic products herd 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, 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 the colour developing of this method is not obvious, be difficult to discernable by eye, visualization of presence cannot detect testing sample.
3, colloid titration method: the method complex operation, is easily 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 without the need to expensive checkout equipment, can the method for on-the-spot visual detection polyhexamethylene guanide content.
Technical scheme of the present invention is: a kind of detection method of polyhexamethylene guanide content, adopts the nano-Au solution of electronegative, particle diameter 13-35nm as indicator, adopts spectrophotometer or colorimetric card to detect polyhexamethylene guanide content as checkout equipment.
The detection method of described polyhexamethylene guanide content, adopts HEPES (hydroxyethyl piperazine ethanesulfonic acid) solution as damping fluid.
The concrete steps of the detection method of described polyhexamethylene guanide content are as follows:
1, standard solution and reagent is prepared: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution.
2, nitrite ion and dilution is prepared:
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: in 93ml water, add 2ml, after the chlorauric acid solution ebuillition of heated of 1%, then adds 5ml, the sodium citrate solution of 1%, continues heating 20 minutes, is cooled to room temperature for subsequent use.
2) secure ph is between 6-8, and HEPES (hydroxyethyl piperazine ethanesulfonic acid) solution of 1mol/L is as damping fluid;
The compound method of HEPES damping fluid is: take 260.39 grams of HEPES and add distilled water dissolving, adjust ph 6 to 8, is settled to 1L.
3) nitrite ion is prepared: by step 1) and 2) obtained nano-Au solution and HEPES damping fluid mix, HEPES solution ultimate density is less than 100mmol/L.
4) prepared and diluted liquid: by step 2) obtained HEPES damping fluid, 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.Concrete steps are as follows:
(1) prepare variable concentrations and gather hexamethyl guanidine standard solution, at least three concentration;
(2) get poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, react 5 minutes;
(3) drawing standard curve: with the light absorption value between wavelength 600 to 700 nanometer of spectrophotometer measurement above-mentioned steps 3-(2) Plays solution, the at least detection of each concentration standard solution three times, average, with polyhexamethylene guanide concentration of standard solution for horizontal ordinate, with the absorptivity of each concentration standard solution for ordinate, drawing standard curve.
(4) get testing sample, add isopyknic nitrite ion, react 5 minutes, with the light absorption value of spectrophotometric determination testing sample between wavelength 600 to 700 nanometer, the typical curve that step 3-(3) draws checks in corresponding concentration value.
Step 3 can also be: adopt the polyhexamethylene guanide concentration in colorimetric card detection testing sample.Specifically:
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, namely concentration color corresponding to close with standard color comparison card tone be the content of polyhexamethylene guanide in testing sample.
In above-mentioned steps a, the method for making of colorimetric card is: the poly-hexamethyl guanidine standard solution of preparation 0.05ppm to 0.5ppm, and at least three concentration, get a standard solution, add isopyknic sample and nitrite ion, mixing, took pictures with digital camera after 5 minutes, after image procossing, colour print.
Principle of the present invention is: in neutral conditions, the nm of gold that the guanidine radicals of poly-hexamethyl guanidine is positively charged with electronegative passes through electrostatic interaction, neutralize the Partial charge in nm of gold, nm of gold is assembled, and produce the distinguishable color change of corresponding naked eyes, the light absorption value of its 600 to 700 nanometers and the content of poly-hexamethyl guanidine proportional, spectrophotometer can be used to realize quantitative detection to polyhexamethylene guanide, colorimetric card can also be used to carry out Visual retrieval.
Beneficial effect of the present invention is:
1, assay method (GB26367-2010) correlativity of the present invention to polyhexamethylene guanide sample tests value and national standard detection method-poly hexamethylene biguanide content is good, and it is good in concentration 0.05-0.5ppm scope internal linear, detection is limited to 0.05ppm, higher than the sensitivity of current bibliographical information.
2, the present invention can both measure poly-six subunit list guanidines and poly-six subunit biguanides, the salt ion not interference measurement of common cationic surfactant, anionic surfactant, non-ionic surfactant, organism and high concentration, 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 cannot detect.
Accompanying drawing explanation
Fig. 1 is the canonical plotting drawn in the present invention;
Fig. 2 is the present invention and national standard detection method correlativity comparison diagram;
Fig. 3 is that the present invention analyzes the test experience figure of thing to difference, and 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 colorimetric card visualization of presence to detect testing sample figure,
Wherein, Fig. 4 the first row is the pattern adopting colorimetric block-regulations provided by the invention to detect poly-six subunit biguanide concentration, second row is the pattern that the colorimetric block-regulations adopting National Standard Method to provide detects poly-six subunit biguanide concentration, and in figure, numeral is the concentration of poly-six subunit biguanides in solution, unit: ppm.
Embodiment
The present invention is illustrated below in conjunction with drawings and Examples.
Embodiment 1:
A detection method for polyhexamethylene guanide content, concrete steps are as follows:
1, standard solution and reagent is prepared: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution.
2, nitrite ion and dilution is prepared:
1) nano-Au solution of anamorphic zone negative charge:
Add in 93ml water 2ml, 1% chlorauric acid solution ebuillition of heated after, then add 5ml, 1% sodium citrate solution, continue heating 20 minutes, be cooled to room temperature for subsequent use.The nano-Au solution of synthesis, electronegative, maximum absorption wavelength is in 520 ± 5 nanometers, and particle diameter is between 13-35 nanometer;
2) secure ph is between 6-8, and HEPES (hydroxyethyl piperazine ethanesulfonic acid) solution of 1mol/L is as damping fluid;
The compound method of HEPES damping fluid is: take 260.39 grams of HEPES and add distilled water dissolving, adjust ph 6 to 8, is settled to 1L.
3) nitrite ion is prepared: by step 1) and 2) obtained nano-Au solution and HEPES damping fluid press 20:1 volume ratio and mix, HEPES solution ultimate density is for being less than 100mmol/L.
4) prepared and diluted liquid: by step 2) obtained HEPES damping fluid, mix by 1:20 volume ratio with distilled water, HEPES solution ultimate density is for being 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) compound concentration is that the series of 0.05-0.5ppm gathers hexamethyl guanidine standard solution, 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, react 5 minutes;
(3) drawing standard curve: with the light absorption value of spectrophotometer measurement above-mentioned steps 3-(2) Plays solution in wavelength 670 nanometer, each concentration standard solution at least detects three times, average, with polyhexamethylene guanide concentration of standard solution for horizontal ordinate, with the absorptivity of each concentration standard solution for ordinate, drawing standard curve, and do linear regression, see Fig. 1, typical curve equation is: y=0.2584x-0.0152 (R
2=0.9999, n=6).
(4) get testing sample, add isopyknic nitrite ion, react 5 minutes, with the light absorption value of spectrophotometer measurement wavelength in 670 nanometers.The typical curve that step (3) is drawn checks in corresponding concentration value.
(5) can be drawn by equation of linear regression, poly-hexamethyl guanidine is linearly good in 0-0.5ppm scope, detects and is limited to 0.05ppm, higher than the sensitivity of current bibliographical information.
Embodiment 2:
The present invention compares with national standard detection method correlativity
(1) compound concentration is that the series of 0.05-0.5ppm gathers hexamethyl guanidine standard solution, 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, react 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 at least detects three times, average, with polyhexamethylene guanide concentration of standard solution for horizontal ordinate, with each absorption of sample rate for ordinate, drawing standard curve, and do linear regression, typical curve equation is: y=0.2584x-0.0152 (R
2=0.9999, n=6).
(4) after getting 20 parts of different Sample Dilutions 1000 times, add the sample after isopyknic dilution and nitrite ion respectively, react 5 minutes, with the light absorption value of spectrophotometer measurement wavelength in 670 nanometers.The typical curve that step (3) is drawn checks in corresponding concentration value, and result is multiplied by 1000 times, be the concentration of sample.
(5) by 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 and compare, 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 used.
Embodiment 3:
Difference is analyzed to the test experience of thing
With poly-six subunit biguanides (PHMB) standard items of 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 analysis thing, sample and nitrite ion ratio by volume 1:9 add, after mixing, the light absorption value at 670nm wavelength measured by sample after 5 minutes, as shown in Figure 3, result shows no matter this kit is poly-six subunit list guanidines, or poly-six subunit biguanides can both measure, and to common cationic surfactant, anionic surfactant, non-ionic surfactant, the salt ion of organism and high concentration all has certain antijamming capability, may be used for the detection of poly-hexamethyl guanidine in 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, took pictures with digital camera after 5 minutes, and after image procossing, colour print makes colorimetric card.Get the sample of six variable concentrations, sample and nitrite ion is added in the ratio of 1:9 in 96 orifice plates, mix, after 5 minutes with standard color comparison card visual colorimetric determination from top to bottom, namely concentration color corresponding to close with standard color comparison card tone be the content of polyhexamethylene guanide in testing sample, its testing result is suitable with setting value, see Fig. 4, show that this law bore hole can differentiate the tone that different concentration gathers hexamethyl guanidine, visualization of presence can detect testing sample, and GB rule is difficult to differentiate.
Claims (7)
1. the detection method of polyhexamethylene guanide content in a polyhexamethylene guanide disinfection sanitizer, it is characterized in that, it adopts the nano-Au solution of electronegative, particle diameter 13-35nm as indicator, adopt spectrophotometer or colorimetric card as checkout equipment, adopt HEPES solution as damping fluid, detect polyhexamethylene guanide content.
2. the detection method of polyhexamethylene guanide content according to claim 1, it is characterized in that, concrete steps are as follows:
1) standard solution and reagent is prepared: gold chloride, sodium citrate, hydroxyethyl piperazine ethanesulfonic acid, distilled water, polyhexamethylene guanide standard solution;
2) nitrite ion and dilution is prepared:
The nano-Au solution of a, anamorphic zone negative charge, its maximum absorption wavelength 520 ± 5nm, particle diameter 13-35nm;
B, secure ph are between 6-8, and HEPES (hydroxyethyl piperazine ethanesulfonic acid) solution of 1mol/L is as damping fluid;
C, preparation nitrite ion: the nano-Au solution obtained by step a and b and the mixing of HEPES damping fluid, HEPES solution ultimate density is less than 100mmol/L;
D, prepared and diluted liquid: the HEPES damping fluid obtained by step b, 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, described step 3) concrete steps as follows:
(1) prepare variable concentrations and gather hexamethyl guanidine standard solution, at least three concentration;
(2) get poly-hexamethyl guanidine standard solution, add isopyknic nitrite ion, react 5 minutes;
(3) drawing standard curve: with the light absorption value between wavelength 600 to 700 nanometer of spectrophotometer measurement above-mentioned steps 3-(2) Plays solution, the at least detection of each concentration standard solution three times, average, with polyhexamethylene guanide concentration of standard solution for horizontal ordinate, with the absorptivity of each concentration standard solution for ordinate, drawing standard curve;
(4) get testing sample, add isopyknic nitrite ion, react 5 minutes, with the light absorption value of spectrophotometric determination testing sample between wavelength 600 to 700 nanometer, the typical curve that step 3-(3) draws checks in corresponding concentration value.
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) production standard 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, namely concentration color corresponding to close with standard color comparison card tone be 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: the poly-hexamethyl guanidine standard solution of preparation 0.05ppm to 0.5ppm, at least three concentration, get a standard solution, add isopyknic sample and nitrite ion, mixing, take pictures with digital camera after 5 minutes, after image procossing, colour print.
6. the detection method of polyhexamethylene guanide content according to claim 2, it is characterized in that, described step 2) compound method of nano-Au solution is in-a: in 93ml water, add 2ml, after the chlorauric acid solution ebuillition of heated of 1%, add 5ml again, the sodium citrate solution of 1%, continues heating 20 minutes, is cooled to room temperature for subsequent use.
7. the detection method of polyhexamethylene guanide content according to claim 2, it is characterized in that, described step 2) compound method of HEPES damping fluid is in-b: take 260.39 grams of HEPES and add distilled water and dissolve, adjust ph 6 to 8, is settled to 1L.
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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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