CN114414674A - Method for detecting active ingredients in citric acid disinfectant - Google Patents

Method for detecting active ingredients in citric acid disinfectant Download PDF

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CN114414674A
CN114414674A CN202111544294.0A CN202111544294A CN114414674A CN 114414674 A CN114414674 A CN 114414674A CN 202111544294 A CN202111544294 A CN 202111544294A CN 114414674 A CN114414674 A CN 114414674A
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acid
solution
citric acid
mother liquor
disinfectant
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董凡
常燕宁
刘磊
张蕊
王蕊
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Jafron Biomedical Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8675Evaluation, i.e. decoding of the signal into analytical information

Abstract

The invention relates to a method for detecting active ingredients in a citric acid disinfectant, which comprises the following steps: step 1: mixing a preset amount of citric acid disinfectant with a first strong base solution, heating, adding a first acidic solution, cooling, transferring to a first volumetric flask, and fixing the volume to obtain a test solution; step 2: detecting peak areas of the effective components in the test solution by high performance liquid chromatography; and step 3: and calculating the content of each effective component of the citric acid disinfectant according to the peak area. The method can more accurately detect the content of the effective components in the disinfectant.

Description

Method for detecting active ingredients in citric acid disinfectant
Technical Field
The invention relates to the technical field of disinfectant detection, in particular to a method for detecting each effective component in citric acid disinfectant.
Background
Hemodialysis is to replace chronic renal failure patients through a hemodialysis machine, in the treatment process, the hemodialysis machine dilutes reverse osmosis water and dialysis concentrated solution into qualified dialysate according to a certain proportion, and the qualified dialysate is dispersed or convected with the blood of the patients through a dialysis membrane in a dialyzer, so that the aims of eliminating toxins in the patients with chronic renal failure, correcting acidosis and improving ion balance are fulfilled. After treatment is finished, the dialysis machine needs to be effectively cleaned and disinfected so as to ensure the treatment safety of dialysis patients and reduce dialysis complications.
At present, most of disinfection liquid used for disinfecting dialysis machines is citric acid disinfection liquid. The citric acid aqueous solution has strong acidity, can remove carbonate precipitated in a dialysis machine pipeline, and has good effect of killing bacterial spores when being heated to the temperature of more than 80 ℃. Therefore, in the disinfection process, the accuracy of the content of the citric acid disinfectant is particularly important for the cleaning and disinfection effects.
The citric acid disinfectant contains various organic acid components including citric acid, lactic acid and malic acid. At present, acid-base titration is mostly adopted for measuring the content of each active ingredient in the citric acid disinfectant, but only the total acid content in the product can be measured by the method, and the content of one acid cannot be determined, so that the method is not beneficial to the quality control of the citric acid disinfectant product. Therefore, a testing method capable of simultaneously and accurately detecting the contents of malic acid, lactic acid and citric acid is needed so as to control the quality of products.
In the prior art, although the detection method disclosed in chinese patent application CN109765309A realizes simultaneous detection of malic acid, lactic acid and citric acid contents, the specificity of lactic acid component cannot be found due to the limitation of detection conditions during the detection process, which may cause deviation of the detection result.
When the citric acid disinfectant is produced, the used lactic acid raw material is high-concentration lactic acid (85-92%), and because the lactic acid molecules contain hydroxyl and carboxyl functional groups, the hydroxyl and the carboxyl of free lactic acid molecules can be polymerized to form lactic anhydride in the production process of the lactic acid raw material; when the concentration of the lactic acid is low, the lactic anhydride in the lactic acid can be gradually hydrolyzed into free lactic acid, and the content of the lactic anhydride is related to the content of the lactic acid, the pH value, the temperature and the like. Therefore, the lactic anhydride component in the produced citric acid disinfectant can be gradually decomposed into free lactic acid along with the prolonging of the product standing time, so that the situation that the total lactic acid content in the citric acid disinfectant is the same but the contents of the lactic anhydride and the free lactic acid are different in different periods can occur, the lactic anhydride and the free lactic acid are not easy to peak or the lactic anhydride is not easy to detect in a liquid phase, and how to more accurately detect the total lactic acid content in the disinfectant is a problem which is faced at present.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for detecting each effective component in a citric acid disinfectant, which can detect the content of each effective component in the disinfectant more accurately.
In order to achieve the purpose of the invention, the invention provides a method for detecting each effective component in citric acid disinfectant, which comprises the following steps:
step 1: mixing a preset amount of citric acid disinfectant with a first strong base solution, heating, adding a first acidic solution, cooling, transferring to a first volumetric flask, and fixing the volume to obtain a test solution;
step 2: detecting peak areas of the effective components in the test solution by high performance liquid chromatography;
and step 3: and calculating the content of each effective component of the citric acid disinfectant according to the peak area.
Therefore, the separation and detection of various organic acid active ingredients in the citric acid disinfectant are realized by the high performance liquid chromatography. According to the invention, the total lactic acid content in the citric acid disinfectant can be more accurately detected by detecting the lactic acid component in the citric acid disinfectant after hydrolysis treatment. The principle of hydrolysis treatment of lactic acid is: lactic anhydride in lactic acid can be gradually hydrolyzed into free lactic acid under the condition of low concentration, but the hydrolysis reaction is slow, and the addition of alkaline substances can promote the hydrolysis reaction and can accelerate the hydrolysis reaction under the condition of heating. Therefore, in the actual production process, in order to conveniently and rapidly detect the product, the invention adopts the scheme of adding alkali into the lactic acid for heating treatment, and uses the acidic solution to adjust the pH value, thereby reducing the interference of the pH value on the detection and improving the detection precision and efficiency.
The further technical proposal is that the first strong alkali solution is one or more alkali solutions selected from sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide and strontium hydroxide; the first acidic solution is a solution of one or more acids selected from sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid and perchloric acid; the number of moles of hydrogen ions of the acid in the first acidic solution and hydroxide ions of the base in the first strong basic solution is the same.
Therefore, the strong base adopted by the hydrolysis treatment of the lactic acid can be the existing hydroxide of alkali metal or alkaline earth metal, the strong inorganic acid or medium strong acid can be adopted for neutralization, the alkali and acid raw materials are easy to obtain, and the detection of the effective components of the organic acid in the citric acid disinfectant is not influenced. The pH is preferably adjusted to the initial state by the coordination of an acid and a base to avoid interference of the pH with the detection.
The further technical scheme is that in the step 1, the heating step is heating to boiling, and the heating time is more than or equal to 4 minutes; the cooling step is cooling to room temperature; the constant volume of the test solution is determined by adopting a mobile phase.
As can be seen from the above, the hydrolysis treatment of lactic acid in the present invention is preferably performed under boiling conditions, so as to maximize the hydrolysis efficiency, the heating time can be, for example, 4 minutes to 10 minutes, the hydrolysis time is short, and the detection efficiency is improved.
The further technical scheme is that the method also comprises the following steps before the step 3: establishing a standard curve of citric acid, malic acid and lactic acid; in step 3, the content of each effective component of the citric acid disinfectant is calculated according to the peak area and the standard curve.
Therefore, the quantitative analysis is preferably carried out by utilizing the standard curve, the content of each effective component of the citric acid disinfectant can be conveniently determined according to the peak area to be detected, the standard curve can be repeatedly applied, and the detection of different citric acid disinfectants is convenient.
The further technical scheme is that the establishment of the standard curve of citric acid, malic acid and lactic acid comprises the following steps: preparing citric acid mother liquor with accurate concentration; preparing malic acid mother liquor with accurate concentration; mixing lactic acid and a second strong base solution, heating, adding a second acidic solution, cooling, and fixing the volume to prepare a lactic acid mother solution with an accurate concentration; preparing a plurality of series of standard solutions with concentration by using citric acid mother liquor, malic acid mother liquor and lactic acid mother liquor, detecting peak areas of citric acid, malic acid and lactic acid in the standard solutions by adopting a high performance liquid chromatography, and establishing standard curves of the citric acid, the malic acid and the lactic acid.
Therefore, when the lactic acid mother solution is prepared, the hydrolysis treatment can be carried out on the lactic acid by adopting the method which is the same as or basically the same as the method for preparing the test solution, so that the lactic anhydride in the lactic acid is promoted to be hydrolyzed, and the accuracy of the standard curve of the lactic acid is improved.
The further technical proposal is that the second alkali solution is respectively selected from one or more alkali solutions of sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide and strontium hydroxide; the second acid solution is respectively selected from one or more acid solutions of sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid and perchloric acid; the number of moles of hydrogen ions of the acid in the second acidic solution and the number of moles of hydroxide ions of the base in the second strong basic solution are the same.
As can be seen from the above, in the preparation of the lactic acid mother liquor according to the present invention, the second strong base solution may be the same as or different from the first strong base solution, and the second acidic solution may be the same as or different from the first acidic solution, as long as the same or substantially the same hydrolysis and neutralization functions can be achieved. Likewise, the pH value is preferably adjusted to the initial state when the mother liquid of lactic acid is prepared, so as to avoid the interference of the pH value on the detection.
The further technical proposal is that when preparing citric acid mother liquor with accurate concentration and malic acid mother liquor with accurate concentration, corresponding organic acid is dissolved by adopting mobile phase and the volume is fixed by adopting mobile phase respectively; when preparing lactic acid mother liquor with accurate concentration and preparing standard solution, respectively adopting mobile phase constant volume.
Therefore, the invention can prepare mother liquor with accurate concentration by fixing the volume in a corresponding volumetric flask. The citric acid and the malic acid are dissolved by adopting a part of mobile phase, transferred into a corresponding volumetric flask and then fixed to the volume by adopting a part of mobile phase. The lactic acid is also transferred to a corresponding second volumetric flask after hydrolysis, and then partial mobile phase is adopted for volume measurement. Preparing standard solution and adopting mobile phase constant volume in corresponding volumetric flask. By adopting the method, the concentration precision of the standard solution can be ensured, so that the precision of the standard curve is ensured.
The further technical scheme is that when the lactic acid mother liquor with accurate concentration is prepared, the heating step is heating to boiling, and the heating time is more than or equal to 4 minutes.
Therefore, when the lactic acid mother solution is prepared, the heating step which is the same as or basically the same as that of the preparation of the test solution can be adopted for heating, so that the hydrolysis efficiency is improved.
The further technical scheme is that the mass ratio of citric acid, malic acid and lactic acid in the same standard solution is 1: 0.1: 0.1.
therefore, the mass ratio of the citric acid, the malic acid and the lactic acid in the same standard solution is preferably determined according to the same or similar proportion of the active ingredients of the conventional citric acid disinfectant, so that the citric acid, the malic acid and the lactic acid in the standard solution can have the mutual relationship among the active ingredients in the citric acid disinfectant, and the standard curve is more accurate.
The further technical scheme is that the mass concentration ratio of the citric acid mother liquor, the malic acid mother liquor and the lactic acid mother liquor is 1: 0.1: 0.1.
therefore, the mass concentration ratio of the citric acid mother liquor, the malic acid mother liquor and the lactic acid mother liquor is preferably determined according to the same or similar proportion of the active ingredients of the conventional citric acid disinfectant, so that the citric acid mother liquor, the malic acid mother liquor and the lactic acid mother liquor with the same volume can be conveniently taken to prepare the standard solution.
The further technical scheme is that in the step 3, the content of each effective component of the citric acid disinfectant is calculated according to the following formula:
Figure BDA0003415319660000061
in the formula, X is the content of each effective component of the citric acid disinfectant,the unit is g/L; c, the concentration of the effective components in the test solution is obtained by a standard curve, and the unit is g/L; v1Is the volume of the test solution, and the unit is L; v2The volume of the citric acid disinfectant solution taken is mL.
Therefore, the concentration of the effective components in the test solution can be obtained according to the peak area and the standard curve, and the content of each effective component in the citric acid disinfectant can be conveniently obtained through calculation according to the concentration.
The further technical scheme is that in the step 2, a chromatographic column adopted by the high performance liquid chromatography is a C18 chromatographic column, the ultraviolet detection wavelength is 210 nm-220 nm, and the mobile phase is a mixed solution of phosphate buffer solution and methanol; or the chromatographic column adopted by the high performance liquid chromatography is a hydrogen type cation exchange chromatographic column, the ultraviolet detection wavelength is 210 nm-220 nm, and the mobile phase is a sulfuric acid solution.
Therefore, the invention can adopt the high-efficiency liquid phase detection condition or other high-efficiency liquid phase detection conditions to detect, different high-efficiency liquid phase detection conditions can detect the citric acid disinfectant, all components can be effectively separated without mutual interference, the diversification of the detection method is realized, the detection results of different detection methods are basically consistent, the deviation is small, and a detector can conveniently select specific high-efficiency liquid phase detection conditions to detect according to the actual conditions of the detector.
Drawings
FIG. 1 is a liquid chromatogram and peak table on a C18 column of untreated lactic acid in examples of the present invention.
FIG. 2 is a liquid chromatogram and peak table of lactic acid on a C18 column after heating with base and pH adjustment with acid in an example of the present invention.
FIG. 3 is a liquid chromatogram and a peak table of untreated lactic acid on a hydrogen cation column in examples of the present invention.
FIG. 4 is a liquid chromatogram and peak table of lactic acid on a hydrogen cation column after heating with base and pH adjustment with acid in an example of the present invention.
FIG. 5 is a liquid chromatogram and a peak table obtained by using a citric acid disinfectant test solution on a C18 chromatographic column in the embodiment of the present invention.
FIG. 6 is a liquid chromatogram and a peak table obtained by subjecting a citric acid disinfectant test solution to a hydrogen-type cation exchange chromatography column in an embodiment of the present invention.
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Detailed Description
Examples
The embodiment comprises the following steps:
1. establishing a standard curve
(1) Preparing lactic acid mother liquor
Preparation of stock solution after lactic acid treatment: 0.50g of lactic acid was precisely weighed, 20mL of a 1mol/L sodium hydroxide solution was added, the mixture was boiled for 5 minutes, and 10mL of a 1mol/L sulfuric acid solution was added. After cooling to room temperature, the solution was transferred to a 100mL volumetric flask and the volume was determined by the mobile phase to prepare a mother solution of lactic acid having a lactic acid content of 5.0 g/L.
The liquid chromatogram and peak table of the treated lactic acid on the C18 column are shown in FIG. 1, and the liquid chromatogram and peak table of the lactic acid treated by the above method on the C18 column are shown in FIG. 2, and it is found that the peak area of the untreated lactic acid is smaller than that of the treated lactic acid on the C18 column under the same concentration condition. Therefore, after the lactic acid is hydrolyzed, the total content of the lactic acid in the product can be detected more accurately.
The liquid chromatogram and the peak table of the untreated lactic acid on the hydrogen-type cation chromatographic column are shown in fig. 3, and the liquid chromatogram and the peak table of the lactic acid with the same concentration on the hydrogen-type cation chromatographic column after being treated by the method are shown in fig. 4. After hydrolysis treatment is carried out on the lactic acid, the lactic acid has a single peak in a liquid phase, and detection of a product is facilitated.
(2) Preparing a citric acid mother solution:
precisely weighing 5.00g of citric acid, adding a mobile phase (less than 100mL), uniformly mixing and dissolving, transferring to a 100mL volumetric flask, and fixing the volume by using the mobile phase to prepare a citric acid mother solution with the citric acid content of 50.0 g/L.
(3) Preparing a malic acid mother solution:
precisely weighing 0.50g of malic acid, adding a mobile phase (less than 100mL), uniformly mixing and dissolving, transferring to a 100mL volumetric flask, and fixing the volume by using the mobile phase to prepare the malic acid mother liquor with the malic acid content of 5.0 g/L.
Any two steps in the steps (1) to (3) can be performed in any sequence, and can also be performed simultaneously.
(4) Preparing standard solution
And (3) preparing the standard solutions containing the citric acid, the malic acid and the lactic acid with six series of concentrations by using the mother liquor prepared in the steps (1) to (3) and using a mobile phase, wherein the standard solutions are respectively 100 mL. The amounts of each mother liquor added and the concentrations of the standard solutions are shown in Table 1 below.
TABLE 1 mother liquor addition and concentration for standard solutions
Figure BDA0003415319660000081
Figure BDA0003415319660000091
(5) Establishing a standard curve
Detecting 6 sets of mixed standard samples with serial concentrations by using a high performance liquid chromatograph, and establishing standard curves of citric acid, malic acid and lactic acid by taking the concentration of each substance as an abscissa and taking a peak area as an ordinate.
2. Detection of content of active ingredients in citric acid disinfectant
(1) Preparing citric acid disinfectant test solution
1.5mL of 20% citric acid disinfectant is taken, 10mL of 1mol/L sodium hydroxide solution is added, the mixture is heated and boiled for 5 minutes, 5mL of 1mol/L sulfuric acid solution is added, the mixture is cooled to room temperature and then transferred to a 100mL volumetric flask, and the volume is fixed to the scale mark by using a mobile phase.
(2) And detecting the detection liquid sample by using a liquid chromatograph, recording peak areas of all substances, and calculating the contents of citric acid, malic acid and lactic acid in the citric acid disinfectant according to a standard curve.
The content of each effective component in the citric acid disinfectant is calculated according to the following formula:
Figure BDA0003415319660000092
wherein, X: the content (g/L) of each active ingredient in the citric acid disinfectant;
c: obtaining the concentration (g/L) of the effective components in the test solution from a linear regression equation of a standard curve;
V1: total volume of test solution (L); in this embodiment V1Is 100mL, namely 0.1L;
V2: volume of citric acid disinfectant taken (mL); in this embodiment V2It was 1.5 mL.
(3) Liquid chromatography conditions during detection
A chromatographic column: a C18 chromatography column; ultraviolet detection wavelength: 210 nm; mobile phase: 0.01mol/L phosphate buffer solution aqueous solution: 90:10 of methanol; flow rate: 0.6 mL/min; column temperature: at 20 ℃. The chromatogram and peak table obtained under the liquid chromatography conditions are shown in fig. 5, in which peak number 1 is malic acid, peak number 2 is lactic acid, and peak number 3 is citric acid.
Or ② chromatographic column: a hydrogen cation exchange chromatography column; ultraviolet detection wavelength: 210 nm; mobile phase: 0.008mol/L sulfuric acid solution; flow rate: 0.6 mL/min; column temperature: 35 ℃ is carried out. The chromatogram and peak table obtained under the liquid chromatography conditions are shown in fig. 6, in which peak number 1 is citric acid, peak number 2 is malic acid, and peak number 3 is lactic acid.
The detection results of the same sample under two chromatographic conditions are shown in the following table 2, and the detection results of the same sample under different chromatographic conditions are close to each other, which shows that the detection method can be applied to different chromatographic conditions. Under different liquid phase detection conditions, the separation degree of each substance can be more than 3, and the separation degree is better.
TABLE 2 test results under different chromatographic conditions
Content of effective component C18 chromatographic column Hydrogen type cation exchange chromatographic column
Citric acid (g/L) 199.5 199.5
Malic acid (g/L) 20.0 19.9
Lactic acid (g/L) 19.3 19.7
Finally, it should be emphasized that the above-described embodiments are merely preferred examples of the invention, which is not intended to limit the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for detecting each effective component in citric acid disinfectant is characterized by comprising the following steps:
step 1: mixing a preset amount of citric acid disinfectant with a first strong base solution, heating, adding a first acidic solution, cooling, transferring to a first volumetric flask, and fixing the volume to obtain a test solution;
step 2: detecting peak areas of the effective components in the test solution by high performance liquid chromatography;
and step 3: and calculating the content of each effective component of the citric acid disinfectant according to the peak area.
2. The method of claim 1, wherein the method comprises the steps of:
the first strong alkali solution is a solution of one or more alkali selected from sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide and strontium hydroxide; the first acidic solution is a solution of one or more acids selected from sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid and perchloric acid; the number of moles of hydrogen ions of the acid in the first acidic solution and hydroxide ions of the base in the first strong alkaline solution is the same.
3. The method of claim 2, wherein the method comprises the steps of:
in the step 1, the heating step is heating to boiling, and the heating time is more than or equal to 4 minutes; the cooling step is cooling to room temperature; the constant volume of the test solution is constant volume by adopting a mobile phase.
4. The method for detecting active ingredients in citric acid disinfectant as claimed in any one of claims 1 to 3, wherein:
before the step 3, the method further comprises the following steps: establishing a standard curve of citric acid, malic acid and lactic acid; in the step 3, the content of each effective component in the citric acid disinfectant is calculated according to the peak area and the standard curve.
5. The method of claim 4, wherein the method comprises the steps of:
establishing a standard curve of citric acid, malic acid and lactic acid comprises the following steps: preparing citric acid mother liquor with accurate concentration; preparing malic acid mother liquor with accurate concentration; mixing lactic acid and a second strong base solution, heating, adding a second acidic solution, cooling, and fixing the volume to prepare a lactic acid mother solution with an accurate concentration; preparing a plurality of series of standard solutions by using the citric acid mother liquor, the malic acid mother liquor and the lactic acid mother liquor, detecting peak areas of citric acid, malic acid and lactic acid in the standard solutions by adopting a high performance liquid chromatography, and establishing a citric acid, malic acid and lactic acid standard curve.
6. The method of claim 5, wherein the method comprises the steps of:
the second strong alkali solution is a solution of one or more alkali selected from sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, barium hydroxide and strontium hydroxide; the second acidic solution is a solution of one or more acids selected from sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid and perchloric acid; the hydrogen ions of the acid in the second acidic solution and the hydroxide ions of the base in the second strong alkaline solution are in the same molar number;
when preparing citric acid mother liquor with accurate concentration and malic acid mother liquor with accurate concentration, respectively adopting mobile phase to dissolve corresponding organic acid and adopting mobile phase to fix volume; when preparing lactic acid mother liquor with accurate concentration and preparing standard solution, respectively adopting mobile phase constant volume;
when the lactic acid mother liquor with accurate concentration is prepared, the heating step is heating to boiling, and the heating time is more than or equal to 4 minutes.
7. The method of claim 5, wherein the method comprises the steps of:
the mass ratio of citric acid to malic acid to lactic acid in the same standard solution is 1: 0.1: 0.1.
8. the method of claim 7, wherein the method comprises the steps of:
the ratio of the mass concentration of the citric acid mother liquor to the mass concentration of the malic acid mother liquor to the mass concentration of the lactic acid mother liquor is 1: 0.1: 0.1.
9. the method of claim 4, wherein the method comprises the steps of:
in the step 3, the content of each effective component of the citric acid disinfectant is calculated according to the following formula:
Figure FDA0003415319650000031
in the formula, X is the content of each effective component of the citric acid disinfectant, and the unit is g/L; c, the concentration of the effective components in the test solution is obtained by a standard curve, and the unit is g/L; v1Is the volume of the test solution, and the unit is L; v2The volume of the citric acid disinfectant solution taken is mL.
10. The method for detecting active ingredients in citric acid disinfectant as claimed in claim 1 or 2, wherein:
in the step 2, the chromatographic column adopted by the high performance liquid chromatography is a C18 chromatographic column, the ultraviolet detection wavelength is 210 nm-220 nm, and the mobile phase is a mixed solution of phosphate buffer solution and methanol; or the chromatographic column adopted by the high performance liquid chromatography is a hydrogen type cation exchange chromatographic column, the ultraviolet detection wavelength is 210 nm-220 nm, and the mobile phase is a sulfuric acid solution.
CN202111544294.0A 2021-12-16 2021-12-16 Method for detecting active ingredients in citric acid disinfectant Pending CN114414674A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105203665A (en) * 2015-09-25 2015-12-30 上海美农生物科技股份有限公司 Method for detecting content of lactic acid in feed acidifier
US20170184555A1 (en) * 2015-12-29 2017-06-29 Waters Technologies Corporation Methods for increasing sensitivity of detection and/or quantification of negatively charged analytes
CN109541124A (en) * 2018-11-27 2019-03-29 新昌和宝生物科技有限公司 The measuring method of lactic anhydride content in a kind of lactic acid
CN109765309A (en) * 2018-12-27 2019-05-17 辽宁三生科技发展有限公司 A kind of method of effective component in separation detection citric acid disinfectant

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105203665A (en) * 2015-09-25 2015-12-30 上海美农生物科技股份有限公司 Method for detecting content of lactic acid in feed acidifier
US20170184555A1 (en) * 2015-12-29 2017-06-29 Waters Technologies Corporation Methods for increasing sensitivity of detection and/or quantification of negatively charged analytes
CN109541124A (en) * 2018-11-27 2019-03-29 新昌和宝生物科技有限公司 The measuring method of lactic anhydride content in a kind of lactic acid
CN109765309A (en) * 2018-12-27 2019-05-17 辽宁三生科技发展有限公司 A kind of method of effective component in separation detection citric acid disinfectant

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱会卷等: "化妆品和消毒剂中α-羟基酸的检测方法比较" *

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