CN105548166B - Test paper for detecting concentration range of o-phthalaldehyde disinfectant - Google Patents
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Abstract
The invention provides a test paper for detecting the concentration range of an o-phthalaldehyde (OPA) disinfectant. The paper is made of oxidized and modified paper pulp, the carboxyl content on the surface of the paper pulp is controlled by adjusting the modification conditions, the paper is treated step by using a solution containing sodium sulfite and phenolphthalein, dried and cut, and the paper is stuck on a bottom plate to prepare the test paper. When in test, the test paper is uniformly changed into red after the test paper is contacted with the disinfectant for 90 seconds, which indicates that the concentration of the o-phthalaldehyde (OPA) reaches the set value of the test paper, otherwise, the test paper is not uniformly or colorless in color change. The test paper controls the carboxyl content on the surface of the fiber through paper pulp modification, can prepare test cards sensitive to different concentration ranges, controls color development through fiber modification, is more uniform and stable than control of soaking solution composition and concentration color development, can meet the requirement on concentration control of the o-phthalaldehyde disinfectant in the disinfection of medical instruments, is simple and convenient to operate, has accurate results, and can quickly and visually evaluate the sterilization condition of the disinfectant.
Description
Technical Field
The invention relates to the field of chemical detection, in particular to test paper for detecting the content of o-phthalaldehyde (OPA) in an OPA disinfectant.
Background
The chemical preparation for killing bacteria is called disinfectant, and the o-phthalaldehyde is a high-level chemical disinfectant newly developed at home and abroad and is approved by FDA in the United states in 1999. In order to ensure the disinfection effect, the concentration of the o-phthalaldehyde in the disinfectant is required to be more than 0.3%, and in practical application, the concentration range of the o-phthalaldehyde in the disinfectant is required to be detected conventionally and rapidly, so that the phenomenon that the concentration is reduced to lose efficacy due to storage or prolonged service time is avoided.
At present, the content detection of the o-phthalaldehyde mainly comprises a titration method, an ultraviolet spectrophotometry method and a high performance liquid chromatography. The titration method refers to a titration test method of glutaraldehyde in the sanitation department's disinfection technical specification' and the 'pharmacopoeia' of China, and the method needs to prepare a plurality of standard solutions, is complicated in steps, consumes time and needs to be completed by professional technicians. Ultraviolet-visible spectrophotometry and chromatographic analysis can be directly used for sampling and analyzing, but both analysis methods require large-scale instruments and equipment and professional operators.
In order to ensure the sterilizing effect of the disinfectant, the concentration range of the o-phthalaldehyde in the disinfectant needs to be judged by a simple and quick method. There has been a report on a glutaraldehyde concentration test card, which tests on the principle that glutaraldehyde reacts with sodium sulfite and amino acid to generate yellow substances, but some users consider that color difference is not easy to distinguish, which may lead to misjudgment.
Disclosure of Invention
The aldehyde group can react with sodium sulfite to generate sodium hydroxide, the sodium hydroxide enables the alkalinity of the system to be increased, the phenolphthalein indicator is changed from colorless to red, the alkalinity of the system is controlled to be increased by introducing the number of carboxyl groups on paper pulp fibers, and the concentration range of aldehyde in the reactant disinfectant is distinguished. The reaction formula is as follows:
R-CHO+ Na2SO3+ 2H2O
RCH(SO3Na)OH + NaOH
therefore, the invention provides a preparation process of the aldehyde disinfectant concentration detection test paper and a use method thereof.
Firstly, the invention provides a preparation method of test paper for detecting the concentration effectiveness of aldehyde disinfectant, which comprises the following steps:
firstly, bleaching softwood sulfate pulp without element chlorine by adopting 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical, NaBr and NaClO for oxidation modification, wherein the adding amount of NaClO is 0.5-4.5 mmol/g;
secondly, filtering, and separating the slurry after oxidation modification;
thirdly, washing the mixture with water to be neutral, and preparing paper for standby, preferably 100g/m2；
Fourthly, soaking: preparing 10-30% sodium sulfite solution and mixing with 0.5-2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor as soaking liquor. Soaking the paper in the solution for 5-30 minutes;
and fifthly, taking out the paper and drying (preferably vacuum at normal temperature).
And sixthly, further cutting the paper, fixing the paper on a non-absorbent substrate by using viscose, and deoxidizing and sealing the paper for later use.
The first step is preferably carried out under the following modification conditions: the concentration of the slurry is 1%, the 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature (15-25 ℃), the pH value of the system is 10-11, the addition amount of NaClO is 0.8mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more.
And correspondingly, in the fourth step, a 10% sodium sulfite solution is prepared and is uniformly mixed with a 1% phenolphthalein absolute ethyl alcohol solution to prepare a mother solution.
This approach can detect: the critical concentration of the o-phthalaldehyde disinfectant is 0.2%, and the test paper can uniformly turn red when the critical concentration is exceeded. When the concentration is less than 0.2%, the color becomes red non-uniform or does not change.
The second preferred mode is modification conditions: concentration of slurry 1%, 0.1mmol/g of 2, 2, 6, 6-tetramethyl piperidone-1-oxyl and 1mmol/g of NaBr are reacted at room temperature (15-25 ℃), pH value of the system is 10-11, NaClO is added in an amount of 2.5mmol/g, and the oxidation reaction is considered to be completed when the pH value is not reduced any more.
And correspondingly, preparing 15% sodium sulfite solution by using the soaking solution, and uniformly mixing the sodium sulfite solution with 1% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
This approach can detect: the critical concentration of the o-phthalaldehyde disinfectant is 0.3%, and the test paper can uniformly turn red when the critical concentration is exceeded. When the concentration is less than 0.3%, the color becomes red non-uniform or does not change.
The third preferred mode is modification conditions: the elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: the slurry is concentrated to 1 percent, 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature (15-25 ℃), the pH value of the system is 10-11, the addition amount of NaClO is 3.1mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more.
And correspondingly, preparing 20% sodium sulfite solution by using the soaking solution, and uniformly mixing the sodium sulfite solution with 2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
This approach can detect: the critical concentration of the o-phthalaldehyde disinfectant is 0.5%, and the test paper can uniformly turn red when the critical concentration is exceeded. When the concentration is less than 0.5%, the color becomes red non-uniform or does not change.
The fourth preferred mode is modification conditions: the elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: the slurry is concentrated to 1 percent, 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature (15-25 ℃), the pH value of the system is 10-11, the addition amount of NaClO is 4.0mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more.
And correspondingly, preparing 30% sodium sulfite solution by using the soaking solution, and uniformly mixing the 30% sodium sulfite solution with 2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
This approach can detect: the critical concentration of the o-phthalaldehyde disinfectant is 0.8%, and the test paper can uniformly turn red when the critical concentration is exceeded. When the concentration is less than 0.8%, the color becomes red non-uniform or does not change.
The invention further provides a method for testing the aldehyde content in the disinfectant by using the test paper, which comprises the following steps:
firstly, removing a toxic agent, adjusting the pH value to 6.5-7.5, and putting the test paper prepared by the invention;
secondly, taking out the test paper after the test paper is completely immersed for 2 to 4 seconds, standing (preferably for 60 to 90 seconds), and observing the color change of the test paper;
judging whether the aldehyde content meets a calibration value according to the color change of the test paper;
if the test paper turns red uniformly, the aldehyde concentration in the disinfectant meets the marking requirement, and if the test paper turns red non-uniformly or does not turn color, the aldehyde concentration in the disinfectant is smaller than the marking value (namely the critical value).
The invention has the advantages that: the test paper controls the carboxyl content on the surface of the fiber through paper pulp modification, and can prepare test cards sensitive to different concentration ranges; the test paper controls color development through fiber modification, and is more uniform and stable in color development compared with control of the composition and concentration of a soaking solution. The test paper disclosed by the invention is simple and convenient to operate, has accurate results, can meet the requirement on the concentration control of the o-phthalaldehyde disinfectant in the disinfection of medical instruments, has no special technical requirement on operators, and can quickly and visually evaluate the sterilization condition of the disinfectant.
Detailed Description
Example 1: the concentration range of the o-phthalaldehyde disinfectant is set to 0.2 percent by using test paper.
Pulp modification
The elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows:the concentration of the slurry is 1%, 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature (15-25 ℃), the pH value of the system is 10-11, the adding amount of NaClO is 0.8mmol/g, when the pH value is not reduced any more, the oxidation reaction is considered to be completed, the oxidized slurry is separated by filtration, washed to be neutral by deionized water, and the slurry is made into 100g/m2The paper is ready for use.
Preparing a soaking solution:
accurately preparing 10% sodium sulfite solution, and uniformly mixing with 1% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
Preparing test paper:
soaking the paper in the solution for 10 min, taking out, vacuum drying at normal temperature, shearing, and fixing on a non-absorbent substrate by using an adhesive, wherein the substrate is a white plastic sheet, so that the test paper for determining the concentration range of the o-phthalaldehyde disinfectant with the critical concentration of 0.2% can be prepared, and the test paper is deoxidized and sealed for storage.
The test paper is used:
taking about 30ml of an o-phthalaldehyde disinfectant, adjusting the pH value to 6.5-7.5, putting the o-phthalaldehyde disinfectant into test paper prepared by the method, taking out the test paper after the test paper is completely immersed for 2 seconds, vertically contacting the test paper with a paper towel, sucking residual liquid, horizontally placing the test paper on the paper towel for 60-90 seconds, and observing the color change of the test paper, wherein the test of the o-phthalaldehyde disinfectant with known concentration shows that the test paper turns uniformly red when the concentration is more than 0.2 percent and turns uniformly red or does not turn uniformly when the concentration is less than 0.2 percent.
Example 2: the concentration range of the o-phthalaldehyde disinfectant is set to 0.3 percent by using test paper.
Pulp modification
The elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: concentrating the slurry to 1%, reacting at room temperature (15-25 deg.C) with 0.1mmol/g of 2, 2, 6, 6-tetramethylpiperidone-1-oxygen free radical and 1mmol/g of NaBr, adjusting the pH value of the system to 10-11, adding 2.5mmol/g of NaClO, determining that the oxidation reaction is completed when the pH value is not reduced any more, filtering to separate the oxidized slurry, washing with deionized water to neutrality, and making into 100g/m2The paper is ready for use.
Preparing a soaking solution:
accurately preparing 15% sodium sulfite solution, and uniformly mixing with 1% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
Preparing test paper:
soaking the paper in the solution for 10 min, taking out, vacuum drying at normal temperature, shearing, and fixing on a non-absorbent substrate by using an adhesive, wherein the substrate is a white plastic sheet, so that the test paper for determining the concentration range of the o-phthalaldehyde disinfectant with the critical concentration of 0.3% can be prepared, and the test paper is deoxidized and sealed for storage.
The test paper is used:
taking about 30ml of an o-phthalaldehyde disinfectant, adjusting the pH value to 6.5-7.5, putting the o-phthalaldehyde disinfectant into test paper prepared by the method, taking out the test paper after the test paper is completely immersed for 2 seconds, vertically contacting the test paper with a paper towel, sucking residual liquid, horizontally placing the test paper on the paper towel for 60-90 seconds, and observing the color change of the test paper, wherein the test of the o-phthalaldehyde disinfectant with known concentration shows that the test paper turns uniformly red when the concentration is more than 0.3 percent and turns uniformly red or does not turn uniformly when the concentration is less than 0.3 percent.
Example 3: the concentration range of the o-phthalaldehyde disinfectant is set to 0.5 percent by using test paper.
Pulp modification
The elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: concentrating the slurry to 1%, reacting at room temperature (15-25 deg.C) with 0.1mmol/g of 2, 2, 6, 6-tetramethylpiperidone-1-oxygen free radical and 1mmol/g of NaBr, adjusting the pH value of the system to 10-11, adding 3.1mmol/g of NaClO, determining that the oxidation reaction is completed when the pH value is not reduced any more, filtering to separate the oxidized slurry, washing with deionized water to neutrality, and making into 100g/m2The paper is ready for use.
Preparing a soaking solution:
accurately preparing 20% sodium sulfite solution, and uniformly mixing with 2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
Preparing test paper:
soaking the paper in the solution for 10 min, taking out, vacuum drying at normal temperature, shearing, and fixing on a non-absorbent substrate by using an adhesive, wherein the substrate is a white plastic sheet, so that the test paper for determining the concentration range of the o-phthalaldehyde disinfectant with the critical concentration of 0.5% can be prepared, and the test paper is deoxidized and sealed for storage.
The test paper is used:
taking about 30ml of an o-phthalaldehyde disinfectant, adjusting the pH value to 6.5-7.5, putting the o-phthalaldehyde disinfectant into test paper prepared by the method, taking out the test paper after the test paper is completely immersed for 2 seconds, vertically contacting the test paper with a paper towel, sucking residual liquid, horizontally placing the test paper on the paper towel for 60-90 seconds, and observing the color change of the test paper, wherein the test of the o-phthalaldehyde disinfectant with known concentration shows that the test paper turns uniformly red when the concentration is more than 0.5 percent and turns uniformly red or does not turn uniformly when the concentration is less than 0.5 percent.
Example 4: the concentration range of the o-phthalaldehyde disinfectant is set to 0.8 percent by using test paper.
Pulp modification
The elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: concentrating the slurry to 1%, reacting at room temperature (15-25 deg.C) with 0.1mmol/g of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical and 1mmol/g of NaBr, adjusting the pH value of the system to 10-11, adding 4.0mmol/g of NaClO, determining that the oxidation reaction is completed when the pH value is not reduced any more, filtering to separate the oxidized slurry, washing with deionized water to neutrality, and making into 100g/m2The paper is ready for use.
Preparing a soaking solution:
accurately preparing 30% sodium sulfite solution, and uniformly mixing with 2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
Preparing test paper:
soaking the paper in the solution for 10 min, taking out, vacuum drying at normal temperature, shearing, and fixing on a non-absorbent substrate by using an adhesive, wherein the substrate is a white plastic sheet, so that the test paper for determining the concentration range of the o-phthalaldehyde disinfectant with the critical concentration of 0.8% can be prepared, and the test paper is deoxidized and sealed for storage.
The test paper is used:
taking about 30ml of an o-phthalaldehyde disinfectant, adjusting the pH value to 6.5-7.5, putting the o-phthalaldehyde disinfectant into test paper prepared by the method, taking out the test paper after the test paper is completely immersed for 2 seconds, vertically contacting the test paper with a paper towel, sucking residual liquid, horizontally placing the test paper on the paper towel for 60-90 seconds, and observing the color change of the test paper, wherein the test of the o-phthalaldehyde disinfectant with known concentration shows that the test paper turns uniformly red when the concentration is more than 0.8 percent and turns uniformly red or does not turn uniformly when the concentration is less than 0.8 percent.
Claims (9)
1. A preparation method of an effectiveness test paper with different critical concentrations for an o-phthalaldehyde disinfectant concentration range is characterized by comprising the following steps:
firstly, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical, NaBr and NaClO are adopted to carry out oxidation modification on elemental chlorine-free bleached softwood kraft pulp, wherein the addition amount of the NaClO is 0.5-4.5 mmol/g;
secondly, filtering, and separating the slurry after oxidation modification;
thirdly, washing the elemental chlorine-free bleached softwood kraft pulp with water to be neutral, and making paper for later use;
fourthly, preparing 10-30% sodium sulfite solution, mixing the sodium sulfite solution with 0.5-2% phenolphthalein absolute ethyl alcohol solution to prepare mother liquor as soaking solution, and soaking the copied paper in the soaking solution;
and fifthly, taking out the paper and drying to obtain the paper.
2. The method of claim 1, wherein: further, the paper is cut and fixed on a non-absorbent substrate by using viscose glue, and then the paper is deoxidized and sealed for standby.
3. The method of claim 1, wherein: the third step is to make 100g/m of paper2(ii) a Fourthly, soaking the paper made into paper in the solution for 5 to 30 minutes; the drying in the fifth step is vacuum drying at normal temperature.
4. The method of claim 1, wherein: the modification conditions in the first step were: the concentration of the slurry is 1%, the concentration of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature, the pH value of the system is 10-11, the addition amount of NaClO is 0.8mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more.
5. The production method according to any one of claims 1 to 3, characterized in that:
the modification conditions in the first step were: the concentration of the slurry is 1%, the concentration of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at room temperature, the pH value of the system is 10-11, the adding amount of NaClO is 0.8mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more;
and in the fourth step, the soaking solution is prepared into 10 percent sodium sulfite solution, and is uniformly mixed with 1 percent phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
6. The production method according to any one of claims 1 to 3, characterized in that:
the modification conditions in the first step were: the concentration of the slurry is 1%, the concentration of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at 15-25 ℃, the pH value of the system is 10-11, the addition amount of NaClO is 2.5mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more;
and in the fourth step, 15% of sodium sulfite solution is prepared as soaking solution, and the soaking solution is uniformly mixed with 1% of phenolphthalein absolute ethyl alcohol solution to prepare mother solution.
7. The production method according to any one of claims 1 to 3, characterized in that:
the modification conditions in the first step were: the elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: the concentration of the slurry is 1%, the concentration of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at 15-25 ℃, the pH value of the system is 10-11, the addition amount of NaClO is 3.1mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more;
and in the fourth step, the soaking solution is prepared into 20 percent sodium sulfite solution, and is uniformly mixed with 2 percent phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
8. The production method according to any one of claims 1 to 3, characterized in that:
the modification conditions in the first step were: the elemental chlorine-free bleached softwood kraft pulp is firstly oxidized and modified by 2, 2, 6, 6-tetramethyl piperidone-1-oxygen radical, NaBr and NaClO, and the modification conditions are as follows: the concentration of the slurry is 1%, the concentration of 2, 2, 6, 6-tetramethyl piperidone-1-oxygen free radical is 0.1mmol/g, NaBr is 1mmol/g, the reaction is carried out at 15-25 ℃, the pH value of the system is 10-11, the addition amount of NaClO is 4.0mmol/g, and the oxidation reaction is considered to be finished when the pH value is not reduced any more;
and in the fourth step, the soaking solution is prepared into 30 percent sodium sulfite solution, and is uniformly mixed with 2 percent phenolphthalein absolute ethyl alcohol solution to prepare mother liquor.
9. Method for testing the aldehyde content of a disinfectant using a test paper obtained by the method according to any one of claims 1 to 8, characterized in that it comprises the following steps:
a detoxifying agent, adjusting pH to 6.5-7.5, placing the test paper obtained by the preparation method of any one of claims 1 to 8;
secondly, taking out the test paper after the test paper is completely immersed for 2 to 4 seconds, standing for 60 to 90 seconds, and observing the color change of the test paper;
and thirdly, judging whether the aldehyde content meets a calibration value according to the color change of the test paper.
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| US10702619B2 (en) * | 2016-05-18 | 2020-07-07 | Asp Global Manufacturing Gmbh | Apparatus and method to measure concentration of disinfectant in medical device reprocessing system |
| CN106323966A (en) * | 2016-10-31 | 2017-01-11 | 百奥森（江苏）食品安全科技有限公司 | Detection paper for disinfector residue and preparation method thereof |
| CN106872459A (en) * | 2017-03-06 | 2017-06-20 | 亳州市新健康科技有限公司 | A kind of OPA thimerosal and Concentration Testing test paper and manufacture craft |
| CN106970075B (en) * | 2017-03-20 | 2019-05-10 | 广西庆荣卫生消毒制品有限公司 | A kind of o-phthalaldehyde Concentration Testing test paper and preparation method thereof |
| CN106970078B (en) * | 2017-05-15 | 2019-10-08 | 北京长江脉医药科技有限责任公司 | A kind of test paper detecting o-phthalaldehyde and its preparation and detection method |
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| CN1477386A (en) * | 2002-08-19 | 2004-02-25 | 杨 柳 | Glutaraldehyde concentration testing card |
| CN103125510A (en) * | 2013-03-22 | 2013-06-05 | 广州市医德生物科技有限责任公司 | Compound phthalic dicarboxaldehyde polyquaternium cationic surface active agent disinfectant and preparation and application thereof |
| CN103994995A (en) * | 2014-05-21 | 2014-08-20 | 德州安捷高科消毒制品有限公司 | Determination method for o-phthalaldehyde |
| CN104677904A (en) * | 2015-02-04 | 2015-06-03 | 北京红辉力上科技有限公司 | Test paper for testing concentration of ortho-phthalaldehyde disinfectant |
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