CN103558174A - Method for measuring content of cresol in lysol by utilizing ultraviolet spectrophotometry - Google Patents

Method for measuring content of cresol in lysol by utilizing ultraviolet spectrophotometry Download PDF

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CN103558174A
CN103558174A CN201310493945.7A CN201310493945A CN103558174A CN 103558174 A CN103558174 A CN 103558174A CN 201310493945 A CN201310493945 A CN 201310493945A CN 103558174 A CN103558174 A CN 103558174A
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lysol
cresols
cresol
ethyl alcohol
absolute ethyl
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CN103558174B (en
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杨雪峰
任秀娟
刘东阳
王清华
韩庆功
张海棠
王自良
胡建和
齐永华
范国英
刘小翠
李珊珊
袁香丽
丁丹霞
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Henan Institute of Science and Technology
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Abstract

The invention discloses a method measuring content of cresol in lysol by utilizing ultraviolet spectrophotometry. According to the key points of the technical scheme, the method is characterized by comprising the following steps: (1) selecting absolute ethyl alcohol as a solvent; (2) absorbing a certain amount of cresol, putting the cresol into a volumetric flask, diluting to achieve the metered volume by taking absolute ethyl alcohol as a solvent, precisely preparing a series concentration of cresol solution as a cresol standard solution, diluting a lysol sample by using the solvent according to the same method, and preparing lysol sample diluents with various concentrations; (3) measuring absorbancy of the cresol standard solution at the measured wavelength by taking absolute ethyl alcohol as a blank solvent, performing linear regression on the absorbancy according to the standard concentration, and establishing a standard curve equation for measuring the content of cresol in lysol; and (4) measuring the absorbancy of the lysol sample diluent at the measured wavelength by taking the absolute ethyl alcohol as a blank solvent, substituting the absorbancy into the standard curve equation, and calculating the concentration of the cresol in lysol. The method has the advantages of simplicity in instrument operation and high detection speed.

Description

A kind of method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol
Technical field:
The present invention relates to sanitizer assay technology, be specifically related to a kind of method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol.
Background technology:
Lysol has another name called cresol solution,saponated, is a kind of traditional phenols environment disinfected agent, is mainly used in the sterilizations such as apparatus, place, mew, excreta.The functional component of Lysol is cresols, and cresols claims again paracresylol, is the potpourri of fractionation obtains from coal tar ortho position, a position and 3 kinds of Cresol Isomeric Compounds of contraposition, and its bactericidal action is stronger, under debita spissitudo, can kill most of reproduction type pathogens.What in Lysol, the content assaying method of cresols adopted conventionally is the vapor-phase chromatography under various chromatographic conditions.For these methods of standard, in the < < Pharmacopoeia of People's Republic of China > > (two) of version in 2005, stipulated sample preparation and the operation steps of the method.But the method exists required gas chromatograph expensive in application process, reagent cost is high, and instrumentation is complicated, and detection time is long, is unsuitable for the shortcomings such as manufacturing enterprise's fast detecting.
In utilizing the process of cresols raw material production Lysol, and in Lysol finished product preservation process, although various standards are in order to determine the content of cresols in Lysol, measured respectively the content of various isomerss, but various standards are not stipulated content or the ratio of each cresols isomers in Lysol, do not need to control respectively ortho position, a position and the separately component ratio of 3 kinds of Cresol Isomeric Compounds of contraposition in system.Therefore, utilize the method for gas chromatography determination cresols content to be more suitable in the quality of production Quality Control to raw materials for production cresols, to produce up-to-standard cresols raw material, and be not suitable for the Fast Measurement that cresols content in process was produced and deposited to Lysol.The method of how using comparatively easy technological means, taking lower testing cost to measure rapidly and accurately cresols content in Lysol is a current difficult problem.
Summary of the invention:
The object of the invention is to design a kind of without expensive instrument, easy and simple to handle, detect fast, result accurately, cresols content assaying method in the Lysol that is easy to promote.
Technical scheme of the present invention is that a kind of method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol, is characterized in that: (1) first selects absolute ethyl alcohol as solvent; (2) a certain amount of cresols of accurate absorption is placed in volumetric flask, with absolute ethyl alcohol, make solvent dilution constant volume, the cresol liquor of accurate configuration series concentration is as cresols standard solution, 4 ℃ save backup, same method, with solvent dilution Lysol sample, precision configures the Lysol sample diluting liquid of various concentration; (3) with absolute ethyl alcohol, do blank solvent, in the absorbance of measuring wavelength place mensuration cresols standard solution, with normal concentration, absorbance is carried out to linear regression, set up the typical curve equation of cresols assay in Lysol; (4) with absolute ethyl alcohol, do blank solvent, in the absorbance of measuring wavelength place mensuration Lysol sample diluting liquid, and substitution typical curve equation, calculate the cresols concentration in lysol.Described cresols standard solution configures by analyzing pure level cresols.Described mensuration wavelength is 278 nm.Although cresols is the potpourri of ortho position, a position and 3 kinds of isomerss of contraposition, but make blank solvent with absolute ethyl alcohol, utilize uv-spectrophotometric instrument to find in 200~400 nm scope interscans, various cresols isomerss all have good uv absorption at detection wavelength 278nm place.Therefore,, according to this ultraviolet absorpting spectrum feature of cresols, the wavelength of determining its assay is 278 nm.
The present invention has the following advantages or good effect:
(1) the present invention, without purchasing expensive instrument, only needs conventional uv-spectrophotometric instrument, and instrumentation is simple, and detection speed is fast, to instrumentation personnel without special technical requirement.
(2) the present invention does not need the special reagents such as the reference substance of various cresols isomerss and special solvent, but the pure level of the analysis that utilizes super quality and competitive price easily to purchase cresols product in contrast, testing cost is cheap, and method is easy to promote.
(3) the present invention does not need to measure respectively the content of various cresols isomerss, can determine the content of cresols in Lysol.
(4) the suitable Fast Measurement that is easy to Lysol production and deposits cresols content in process of the present invention.
Accompanying drawing explanation:
Fig. 1 is the ultraviolet absorpting spectrum that adopts the cresols standard solution that method obtains described in embodiment,
Fig. 2 is the typical curve equation that adopts cresols assay in the Lysol that method is set up described in embodiment.
Embodiment:
describe embodiment in detail,
(1) the accurate pure level of a certain amount of analysis cresols of drawing is placed in volumetric flask, with absolute ethyl alcohol, makes solvent dilution constant volume, and the cresol liquor of accurate configuration series concentration is as cresols standard solution, and 4 ℃ save backup.Same method, with absolute ethyl alcohol dilution Lysol sample, precision configures Lysol sample diluting liquid, and 4 ℃ save backup.
(2) using absolute ethyl alcohol as blank solvent, at 278 nm places, measure the absorbance of cresols standard solution, with normal concentration (C), absorbance (A) is carried out to linear regression, set up the typical curve equation of cresols assay in Lysol.
(3) using absolute ethyl alcohol as blank solvent, measure after the absorbance of Lysol sample diluting liquid at 278 nm places, substitution typical curve equation, calculates the cresols concentration in lysol.
For further illustrating concrete result of use of the present invention, below adopt test figure to be verified.
the foundation of test example 1 typical curve equation
According to embodiment, the accurate pure level of a certain amount of analysis cresols of drawing is placed in volumetric flask, with absolute ethyl alcohol, make solvent dilution constant volume, the solution that accurate configuration cresols concentration is respectively 0.005,0.008,0.01,0.02,0.03,0.04 and 0.05 μ L/mL is as cresols standard solution, and 4 ℃ save backup.
With absolute ethyl alcohol, make blank solvent, at 278 nm places, measure respectively the absorbance (A) of each cresols standard solution, with reference substance concentration (C), A is carried out to linear regression, the typical curve equation of setting up cresols assay in Lysol is: A=19.076C+0.0006(R 2=0.9996, n=10), cresols concentration well (is shown in Figure of description, Fig. 2) in 0.005~0.05 uL/mL scope internal linear relation.The detection of the method is limited to 0.0006 uL/mL.
test example 2 precision tests
Get the Lysol sample diluting liquid of same lot number, in 6 absorbances of 278 nm place replications, calculate relative standard deviation (RSD), test findings is in Table 1.As shown in Table 1, precision test RSD is 1.66%, is less than 2.0%, shows that the precision of the method is high.
Table 1 Precision test result
Figure 2013104939457100002DEST_PATH_IMAGE002
test example 3 replica tests
6 parts of the identical Lysol sample diluting liquids of compound concentration, measure respectively absorbance at 278 nm places, calculate relative standard deviation (RSD), and test findings is in Table 2.As shown in Table 2, the RSD of replica test result is 1.71%, is less than 2.0%, shows that the repeatability of the method is good.
Table 2 replica test result
test example 4 recovery tests
Get concentration known and be 3 parts of the Lysol sample diluting liquids of 0.01uL/mL, adding respectively concentration is the cresols standard solution of 0.005,0.01 and 0.03 uL/mL, then at 278 nm wavelength places, measure absorbance, by calibrating curve equation, calculate measured value, according to average recovery=(measured value after application of sample-known test liquid content)/reference substance content * 100% formula, calculate recovery rate, average recovery rate and relative standard deviation (RSD), test findings is in Table 3.The average recovery rate of 3 kinds of concentration solution is 100.89(± 1.65) %, RSD is 1.64%.
Table 3 recovery test result (n=3)
test example 5 sample sizes are measured
According to < < Pharmacopoeia of People's Republic of China > > version (two) in 2005, prepare respectively the Lysol sample of 3 batches, and be diluted to Lysol sample diluting liquid by absolute ethyl alcohol precision, at 278 nm wavelength places, measure absorbance, substitution typical curve equation, calculates cresols content and labelled amount in lysol sample.Result shows, utilizes the cresols labelled amount result of the method mensuration and the < < Pharmacopoeia of People's Republic of China > > middle cresols labelled amount result requiring of version (two) in 2005 consistent.

Claims (3)

1. a method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol, is characterized in that: (1) first selects absolute ethyl alcohol as solvent; (2) a certain amount of cresols of accurate absorption is placed in volumetric flask, with absolute ethyl alcohol, make solvent dilution constant volume, the cresol liquor of accurate configuration series concentration is as cresols standard solution, 4 ℃ save backup, same method, with solvent dilution Lysol sample, the Lysol sample diluting liquid of the various concentration of accurate configuration; (3) with absolute ethyl alcohol, make blank solvent, in the absorbance of measuring wavelength place mensuration cresols standard solution, with normal concentration, absorbance is carried out to linear regression, set up the typical curve equation of cresols assay in Lysol; (4) with absolute ethyl alcohol, make blank solvent, in the absorbance of measuring wavelength place mensuration Lysol sample diluting liquid, and substitution typical curve equation, calculate the cresols concentration in lysol.
2. a kind of method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol as claimed in claim 1, is characterized in that: described cresols standard solution configures by analyzing pure level cresols.
3. a kind of method of utilizing cresols content in determined by ultraviolet spectrophotometry Lysol as claimed in claim 1, is characterized in that: described mensuration wavelength is 278 nm.
CN201310493945.7A 2013-10-21 2013-10-21 A kind of method utilizing cresol content in determined by ultraviolet spectrophotometry Lysol Expired - Fee Related CN103558174B (en)

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CN109444065A (en) * 2018-12-21 2019-03-08 天津利海石化有限公司 The measuring method of phenol content in by-product concentrated hydrochloric acid
CN109752336A (en) * 2017-11-05 2019-05-14 镇江华维检测技术有限公司 Detect the foundation of the ultraviolet spectrophotometry of o-phenyl phenol content
CN114047155A (en) * 2021-09-26 2022-02-15 嘉必优生物技术(武汉)股份有限公司 Method for rapidly detecting carotenoid

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Publication number Priority date Publication date Assignee Title
CN109752336A (en) * 2017-11-05 2019-05-14 镇江华维检测技术有限公司 Detect the foundation of the ultraviolet spectrophotometry of o-phenyl phenol content
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CN114047155A (en) * 2021-09-26 2022-02-15 嘉必优生物技术(武汉)股份有限公司 Method for rapidly detecting carotenoid

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