CN117849231A - Liquid phase detection method for content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride - Google Patents
Liquid phase detection method for content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 52
- 239000007791 liquid phase Substances 0.000 title claims abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 29
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 25
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 25
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 25
- 239000012071 phase Substances 0.000 claims abstract description 23
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 70
- 235000019270 ammonium chloride Nutrition 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 9
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract description 21
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000011550 stock solution Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000012224 working solution Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 238000007865 diluting Methods 0.000 description 5
- 238000003556 assay Methods 0.000 description 4
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 239000000645 desinfectant Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- -1 sodium tetraphenylborate Chemical compound 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000003260 vortexing Methods 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 229960002233 benzalkonium bromide Drugs 0.000 description 2
- 229960000686 benzalkonium chloride Drugs 0.000 description 2
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 description 2
- XIWFQDBQMCDYJT-UHFFFAOYSA-M benzyl-dimethyl-tridecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 XIWFQDBQMCDYJT-UHFFFAOYSA-M 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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Abstract
The invention provides a liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, which belongs to the technical field of chemical detection and comprises high performance liquid chromatography determination, wherein the chromatographic conditions of the high performance liquid chromatography determination are that a chromatographic column is C18, the specification of the chromatographic column is 4.6mm, 250mm, a mobile phase is that an ammonium acetate solution is mixed with a methanol solution, and the concentration ratio of the ammonium acetate solution to the methanol solution is 11% -89% -13% -87%. The invention provides a liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, which has high realization sensitivity and low detection limit, and is suitable for the liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in mixed quaternary ammonium salt.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride.
Background
C12-14-alkyl dimethyl ethyl benzyl ammonium chloride belongs to a quaternary ammonium salt, is also a cationic surfactant, and belongs to a non-oxidizing bactericide. It can be used as sludge remover, and also can be used as mildew inhibitor, antistatic agent, emulsifying agent and modifying agent in textile and dyeing fields. Because the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride has the characteristics of sterilization and corrosion resistance, the antibacterial agent can be added into wet tissues as an antibacterial agent.
The method A.4 in the annex of GB/T26369-2020 hygienic requirement for Quaternary ammonium salt disinfectant in the quaternary ammonium salt is four: sodium tetraphenylborate titration. The content of the quaternary ammonium salt was determined by measuring the cation (bactericidal active ingredient) in the quaternary ammonium salt. In an aqueous alkaline solution, the positively charged quaternary ammonium salt interacts with the negatively charged bromophenol blue acidic fuel indicator to form a blue ion-pair compound which is readily soluble in water-immiscible chloroform. Because this blue compound is less stable than the compound formed between sodium tetraphenylborate and the quaternary ammonium salt, bromophenol blue is used as an indicator for titrating the quaternary ammonium salt with sodium tetraphenylborate by taking advantage of this property. At the beginning of the titration, the quaternary ammonium salt was combined with bromophenol blue to give a blue compound. When titration is carried out to near end point, bromophenol blue indicator is gradually replaced by sodium tetraphenylboron from blue compound and is released, and is transferred into alkaline water layer due to insolubility in chloroform, under intense shaking, blue color of chloroform layer is resolved and alkaline water layer is light purple, which is the end point. The application range is as follows: the cationic portions of the benzalkonium bromide, benzalkonium chloride or other anionically substituted quaternary ammonium salts are the same, and the method is suitable for measuring the content of benzalkonium bromide in raw materials or single chemical disinfectants, and is also suitable for measuring the content of benzalkonium chloride or other anionically substituted quaternary ammonium salts in raw materials or single chemical disinfectants. The detection limit of the method is 0.9g/L.
However, the detection method has low sensitivity and higher detection limit, and is not suitable for detecting the mixed quaternary ammonium salt raw materials of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride and the compounded wet towel liquid containing the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride. Therefore, it is necessary to provide a liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, so as to solve the problems that the detection method has low sensitivity and high detection limit and is not suitable for detecting the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in mixed quaternary ammonium salt.
Disclosure of Invention
In view of the above, the invention provides a liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, which has high realization sensitivity and low detection limit, and is suitable for the liquid phase detection method for the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in mixed quaternary ammonium salt.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride comprises high performance liquid chromatography determination, wherein the chromatographic conditions of the high performance liquid chromatography determination are that a chromatographic column is C18, the specification of the chromatographic column is 4.6mm, 250mm, a mobile phase is that an ammonium acetate solution is mixed with a methanol solution, and the concentration ratio of the ammonium acetate solution to the methanol solution is 11% -89% -13% -87%.
By using ammonium acetate and methanol as mobile phases, the cost of liquid chromatography measurement is reduced, and a detection method capable of detecting the content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in the mixed quaternary ammonium salt is established. The detection method has high sensitivity, the detection limit is 10mg/L, and the quantitative limit is 30mg/L.
Optionally, the flow rate of the mobile phase is 0.8-1.2 mL/min.
Optionally, the flow rate of the mobile phase is 1mL/min.
Optionally, the sample injection amount in the high performance liquid chromatography measurement step is 20 μl.
Optionally, the concentration of the ammonium acetate solution is 0.1mol/L.
Optionally, the ammonium acetate solution is adjusted to a pH of 5 using an acidic agent.
Optionally, the acidic agent is glacial acetic acid.
Optionally, the column temperature of the chromatographic column ranges from 20 ℃ to 30 ℃.
Alternatively, the column temperature of the chromatographic column is 25 ℃.
Optionally, the detection wavelength in the high performance liquid chromatography determination step is 269nm.
The technical scheme of the invention at least comprises the following beneficial effects:
the liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride provided by the invention has the detection limit of 10mg/L, has high sensitivity and low cost, and is suitable for the liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in the mixed quaternary ammonium salt, and the detection result in the embodiment shows that the error is small.
Drawings
FIG. 1 is a graph of the standard operation of a C12-14-alkyldimethylethylbenzyl ammonium chloride in an example of the present invention;
FIG. 2 is a high performance liquid chromatography of sample one of example 1 of the present invention;
FIG. 3 is a high performance liquid chromatography of sample two in example 2 of the present invention;
FIG. 4 is a high performance liquid chromatography of sample three in example 3 of the present invention;
FIG. 5 is a high performance liquid chromatography of sample four in example 4 of the present invention;
FIG. 6 is a high performance liquid chromatography of the C12-C14-alkyldimethylethylbenzyl ammonium chloride standard of Experimental example 1 of the present invention;
FIG. 7 is a high performance liquid chromatography of the C12-C14-alkyldimethylethylbenzyl ammonium chloride standard of Experimental example 2 of the present invention;
FIG. 8 is a high performance liquid chromatography of the C12-C14-alkyldimethylethylbenzyl ammonium chloride standard of Experimental example 3 of the present invention;
FIG. 9 is a UV scan of a C12-C14-alkyldimethylethylbenzyl ammonium chloride standard in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 9 of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which are obtained by a person skilled in the art based on the described embodiments of the invention, fall within the scope of protection of the invention.
The main reagents and instruments used in the examples of the present invention:
standard substance: c12-14-alkyl dimethyl ethyl benzyl ammonium chloride standard (content > 99%)
Reagent: methanol (chromatographic purity); ammonium acetate (chromatographic purity); glacial acetic acid (chromatographic purity); the experimental water meets the specification of GB/T6682-2008 three-level water (distilled water or deionized water or water with equivalent purity)
Instrument: the high performance liquid chromatograph is provided with a diode array detector; an analytical balance; an ultrasonic cleaner; a vortex oscillator.
Example 1
Preparing a mobile phase: 7.708g of ammonium acetate was dissolved in 1L of water, mixed well and glacial acetic acid was added to adjust the pH=5.00.
Preparation of standard stock solution: 100mg of C12-14-alkyldimethylethylbenzyl ammonium chloride was weighed, dissolved in methanol and fixed to a volume of 100mL to give 1.0g/L standard stock solution.
Preparation of a standard series: and respectively transferring 1mL, 2mL, 4mL, 6mL and 8mL of stock solution, placing the stock solution into a 10mL volumetric flask, diluting with water, fixing the volume to a scale, shaking uniformly for later use, and respectively obtaining the corresponding working solution with mass concentrations of 100mg/L, 200mg/L, 400mg/L, 600mg/L and 800mg/L.
And (3) manufacturing a standard curve: the response value of the standard series of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is measured under the condition of a specified liquid chromatograph according to the order of low mass concentration. And (3) taking the mass concentration of the working solution as an abscissa and the sum of corresponding peak areas as an ordinate to manufacture a standard curve, which is shown in figure 1.
Sample treatment: sample one was removed, placed in a 10mL volumetric flask, diluted with water to volume, vortexed with a vortexing shaker, and filtered through a 0.45um filter membrane. The sample I contains mixed quaternary ammonium salt, the configuration content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride of the sample I is 80.2 percent, and the sample I is detected by high performance liquid chromatography to obtain the figure 2.
High performance liquid chromatography assay
After the instrument is stable, the treated samples are sequentially injected into the chromatographic column under the given instrument conditions.
The chromatographic conditions are as follows: chromatographic column: c18,4.6mm×250mm,5 μm;
column temperature: 25 ℃;
detection wavelength: 269nm;
sample injection amount: 20. Mu.L;
flow rate: 1mL/min;
mobile phase: 0.1mol/L ammonium acetate solution (pH=5.0) methanol=11%: 89%;
content calculation
The content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is calculated according to the following formula:
wherein:
x represents the total content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, and the unit is; ρ represents the total mass concentration of C12-14-alkyldimethylethylbenzyl ammonium chloride in mg/L in the sample calculated by the standard curve; v represents the constant volume of the sample, and the unit is mL; m represents the sample sampling amount, and the unit is g. The sample-C12-14-alkyldimethylethylbenzyl ammonium chloride content was calculated to be 80.19% according to the substitution of FIG. 2.
The measured value was 0.01% different from the actual value by 80.19% in terms of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride measured in sample one, which was 80.2% in sample one.
According to the liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, provided by the invention, the cost of liquid chromatography determination is reduced by using the ammonium acetate and the methanol as mobile phases, and the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in the mixed quaternary ammonium salt can be detected.
Example 2
Preparing a mobile phase: 7.708g of ammonium acetate was dissolved in 1L of water, mixed well and glacial acetic acid was added to adjust the pH=5.00.
Preparation of standard stock solution: 100mg of C12-14-alkyldimethylethylbenzyl ammonium chloride was weighed, dissolved in methanol and fixed to a volume of 100mL to give 1.0g/L standard stock solution.
Preparation of a standard series: and respectively transferring 1mL, 2mL, 4mL, 6mL and 8mL of stock solution, placing the stock solution into a 10mL volumetric flask, diluting with water, fixing the volume to a scale, shaking uniformly for later use, and respectively obtaining the corresponding working solution with mass concentrations of 100mg/L, 200mg/L, 400mg/L, 600mg/L and 800mg/L.
And (3) manufacturing a standard curve: the response value of the standard series of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is measured under the condition of a specified liquid chromatograph according to the order of low mass concentration. And (3) taking the mass concentration of the working solution as an abscissa and the sum of corresponding peak areas as an ordinate to manufacture a standard curve, which is shown in figure 1.
Sample treatment: sample two was removed, placed in a 10mL volumetric flask, diluted with water to volume, vortexed with a vortexing shaker, and filtered through a 0.45um filter membrane. The sample II contains mixed quaternary ammonium salt, the preparation content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride of the sample II is 80.0%, and the sample II is detected by high performance liquid chromatography to obtain the figure 3.
High performance liquid chromatography assay
After the instrument is stable, the treated samples are sequentially injected into the chromatographic column under the given instrument conditions.
The chromatographic conditions are as follows: chromatographic column: c18,4.6mm×250mm,5 μm;
column temperature: 25 ℃;
detection wavelength: 269nm;
sample injection amount: 20. Mu.L;
flow rate: 1mL/min;
mobile phase: 0.1mol/L ammonium acetate solution (ph=5.0) methanol=12%: 88%;
content calculation
The content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is calculated according to the following formula:
wherein:
x represents the total content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, and the unit is; ρ represents the total mass concentration of C12-14-alkyldimethylethylbenzyl ammonium chloride in mg/L in the sample calculated by the standard curve; v represents the constant volume of the sample, and the unit is mL; m represents the sample sampling amount, and the unit is g. The sample di-C12-14-alkyldimethylethylbenzyl ammonium chloride content was calculated as 80.03% according to the substitution of FIG. 3.
The measured value was 0.03% different from the actual value and the error was 0.0375% based on the measured content of C12-14-alkyldimethylethylbenzyl ammonium chloride in sample two being 80.03% and the content of C12-14-alkyldimethylethylbenzyl ammonium chloride in sample two being 80.0% when being prepared.
Example 3
Preparing a mobile phase: 7.708g of ammonium acetate was dissolved in 1L of water, mixed well and glacial acetic acid was added to adjust the pH=5.00.
Preparation of standard stock solution: 100mg of C12-14-alkyldimethylethylbenzyl ammonium chloride was weighed, dissolved in methanol and fixed to a volume of 100mL to give 1.0g/L standard stock solution.
Preparation of a standard series: and respectively transferring 1mL, 2mL, 4mL, 6mL and 8mL of stock solution, placing the stock solution into a 10mL volumetric flask, diluting with water, fixing the volume to a scale, shaking uniformly for later use, and respectively obtaining the corresponding working solution with mass concentrations of 100mg/L, 200mg/L, 400mg/L, 600mg/L and 800mg/L.
And (3) manufacturing a standard curve: the response value of the standard series of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is measured under the condition of a specified liquid chromatograph according to the order of low mass concentration. And (3) taking the mass concentration of the working solution as an abscissa and the sum of corresponding peak areas as an ordinate to manufacture a standard curve, which is shown in figure 1.
Sample treatment: and transferring the third sample, placing the third sample into a 10mL volumetric flask, diluting with water to a fixed volume, mixing uniformly by vortex by a vortex oscillator, and filtering by a 0.45um filter membrane. Sample three is a compound wet towel liquid containing C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, the preparation content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride of the sample three is 1.137%, and the sample three is detected by high performance liquid chromatography to obtain the figure 4.
High performance liquid chromatography assay
After the instrument is stable, the treated samples are sequentially injected into the chromatographic column under the given instrument conditions.
The chromatographic conditions are as follows: chromatographic column: c18,4.6mm×250mm,5 μm;
column temperature: 25 ℃;
detection wavelength: 269nm;
sample injection amount: 20. Mu.L;
flow rate: 1mL/min;
mobile phase: 0.1mol/L ammonium acetate solution (ph=5.0) methanol=13%: 87%;
content calculation
The content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is calculated according to the following formula:
wherein:
x represents the total content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, and the unit is; ρ represents the total mass concentration of C12-14-alkyldimethylethylbenzyl ammonium chloride in mg/L in the sample calculated by the standard curve; v represents the constant volume of the sample, and the unit is mL; m represents the sample sampling amount, and the unit is g. The tri-C12-14-alkyldimethylethylbenzyl ammonium chloride content of the sample was calculated to be 1.14% according to the substitution of FIG. 4.
The measured value was 0.003% different from the actual value by 1.14% in terms of the C12-14-alkyldimethylethylbenzyl ammonium chloride content in sample three, and the C12-14-alkyldimethylethylbenzyl ammonium chloride content in sample three was 1.137% in terms of the configuration, with an error of 2.7%.
Example 4
Preparing a mobile phase: 7.708g of ammonium acetate was dissolved in 1L of water, mixed well and glacial acetic acid was added to adjust the pH=5.00.
Preparation of standard stock solution: 100mg of C12-14-alkyldimethylethylbenzyl ammonium chloride was weighed, dissolved in methanol and fixed to a volume of 100mL to give 1.0g/L standard stock solution.
Preparation of a standard series: and respectively transferring 1mL, 2mL, 4mL, 6mL and 8mL of stock solution, placing the stock solution into a 10mL volumetric flask, diluting with water, fixing the volume to a scale, shaking uniformly for later use, and respectively obtaining the corresponding working solution with mass concentrations of 100mg/L, 200mg/L, 400mg/L, 600mg/L and 800mg/L.
And (3) manufacturing a standard curve: the response value of the standard series of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is measured under the condition of a specified liquid chromatograph according to the order of low mass concentration. And (3) taking the mass concentration of the working solution as an abscissa and the sum of corresponding peak areas as an ordinate to manufacture a standard curve, which is shown in figure 1.
Sample treatment: sample four was removed, placed in a 10mL volumetric flask, diluted with water to volume, vortexed with a vortexing shaker, and filtered through a 0.45um filter membrane. Sample three is a compound wet towel liquid containing C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, the preparation content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride of sample four is 0.616%, and the figure 5 is obtained after high performance liquid chromatography detection.
High performance liquid chromatography assay
After the instrument is stable, the treated samples are sequentially injected into the chromatographic column under the given instrument conditions.
The chromatographic conditions are as follows: chromatographic column: c18,4.6mm×250mm,5 μm;
column temperature: 25 ℃;
detection wavelength: 269nm;
sample injection amount: 20. Mu.L;
flow rate: 1mL/min;
mobile phase: 0.1mol/L ammonium acetate solution (ph=5.0) methanol=12%: 88%;
content calculation
The content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is calculated according to the following formula:
wherein:
x represents the total content of C12-14-alkyl dimethyl ethyl benzyl ammonium chloride, and the unit is; ρ represents the total mass concentration of C12-14-alkyldimethylethylbenzyl ammonium chloride in mg/L in the sample calculated by the standard curve; v represents the constant volume of the sample, and the unit is mL; m represents the sample sampling amount, and the unit is g. The sample tetra-C12-14-alkyldimethylethylbenzyl ammonium chloride content was calculated to be 0.61% according to the substitution of FIG. 5.
The C12-14-alkyldimethylethylbenzyl ammonium chloride content was 0.61% as measured in sample four, whereas the C12-14-alkyldimethylethylbenzyl ammonium chloride content was 0.616% in sample four configuration, and the measured value was 0.006% different from the actual value, with an error of 0.98%.
As can be seen from examples 1-2, the detection method provided by the invention has the advantages that the detection errors of the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in the mixed quaternary ammonium salt are respectively 0.013% and 0.0375%, the average error is 0.02525%, the error is small, and the sensitivity is high.
As can be seen from examples 3-4, the detection method provided by the invention has the advantages that the detection errors of the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride in the compounded wet tissue liquid are respectively 2.7% and 0.98%, the average error is 1.84%, the error is smaller, and the sensitivity is higher.
Experiment on influence of proportion of mobile phase on high performance liquid chromatography
Experiment 1
A high performance liquid chromatography was performed on a C12-C14-alkyldimethylethylbenzyl ammonium chloride standard, and the chromatographic conditions were the same as in example 4, giving FIG. 6.
Experiment 2
High performance liquid chromatography was performed on a standard of C12-C14-alkyldimethylethylbenzyl ammonium chloride, the chromatographic conditions differing from experiment 1 only in the mobile phase ratio of 0.1mol/L ammonium acetate solution (ph=5.00): methanol (15%: 85%) to yield fig. 7.
Experiment 3
High performance liquid chromatography was performed on a standard of C12-C14-alkyldimethylethylbenzyl ammonium chloride, the chromatographic conditions differing from experiment 1 only in the mobile phase ratio of 0.1mol/L ammonium acetate solution (ph=5.00): methanol (10%: 90%) to yield fig. 8.
Diode array detection was performed on the C12-C14-alkyldimethylethylbenzyl ammonium chloride standard to give FIG. 9.
As can be seen from fig. 6, 7 and 8 obtained in experiments 1, 2 and 3, the peak shape separation effect is good, the response effect is good, and the required time is proper; FIG. 7 shows that the peak time is late, the peak shape is wide, resulting in a lower response value and longer run time of the method; fig. 8 shows that the peak shapes overlap and no calculation can be performed. Whereas experiments 1, 2, 3 differ only in the proportion of mobile phase, it is therefore known that the proportion of mobile phase has a significant effect on the detection of the content of C12-C14-alkyldimethylethylbenzyl ammonium chloride and in ammonium acetate solution: methanol 11%:89% -13%: the detection effect is best between 87%. The proportion of mobile phase selected in the present invention is therefore in the range of ammonium acetate solution: methanol 11%:89% -13%: 87%.
As can be seen from FIG. 9, C12-C14-alkyldimethylethylbenzyl ammonium chloride can select 269nm as the detection wavelength.
The foregoing is a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride is characterized by comprising high performance liquid chromatography determination, wherein the chromatographic conditions of the high performance liquid chromatography determination are that a chromatographic column is C18, the specification of the chromatographic column is 4.6mm, 250mm, a mobile phase is formed by mixing an ammonium acetate solution and a methanol solution, and the concentration ratio of the ammonium acetate solution to the methanol solution is 11% -89% -13% -87%.
2. The liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride according to claim 1, wherein the flow rate of the mobile phase is 0.8-1.2 mL/min.
3. The method for liquid phase detection of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride according to claim 1, wherein the flow rate of the mobile phase is 1mL/min.
4. The liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride according to claim 1, wherein the sample injection amount in the high performance liquid chromatography determination step is 20 mu L.
5. The liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride according to claim 1, wherein the concentration of the ammonium acetate solution is 0.1mol/L.
6. The method for liquid phase detection of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride according to claim 1, characterized in that the ammonium acetate solution is adjusted to pH 5 using an acidic agent.
7. The method for liquid phase detection of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride according to claim 6, wherein the acidic agent is glacial acetic acid.
8. The liquid phase detection method for the content of the C12-14-alkyl dimethyl ethyl benzyl ammonium chloride according to claim 1, wherein the column temperature of the chromatographic column ranges from 20 ℃ to 30 ℃.
9. The method for liquid phase detection of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride according to claim 8, wherein the column temperature of the chromatographic column is 25 ℃.
10. The method for liquid phase detection of the content of C12-14-alkyldimethylethylbenzyl ammonium chloride according to claim 1, wherein the detection wavelength in the high performance liquid chromatography measurement step is 269nm.
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