CN110618230A - Method for detecting dodecyl paraben - Google Patents
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Abstract
The invention discloses a method for detecting dodecyl paraben, which adopts high performance liquid chromatography to detect the content of dodecyl paraben or substances containing the dodecyl paraben and comprises the following steps of: 1) preparing a standard solution; 2) detecting the standard solution; 3) drawing a standard curve; 4) and (5) measuring the content of the sample. The method adopts a high performance liquid chromatograph to detect the dodecyl paraben, adopts an external standard method to carry out quantitative analysis, thereby determining the content of the dodecyl paraben in the sample, has high precision, high accuracy and good repeatability, can realize direct detection of the sample, greatly reduces the analysis time, is simple, easy, convenient and reliable, and reduces unnecessary complex operations such as concentration and extraction. Meanwhile, the chromatographic conditions adopted by the method have small influence on the aspects of the separation degree, the peak shape, the symmetry degree and the like of the sample, and the dodecyl paraben can be well separated.
Description
Technical Field
The invention belongs to the technical field of analysis, and particularly relates to a method for detecting dodecyl paraben.
Background
The nipagin ester is an organic chemical mildew-proof preservative, is synthesized by a chemical method, and is a safe and efficient preservative adopted internationally. Nipagin ester (p-hydroxybenzoate ester, molecular formula p-HOC)6H4CO2R) its antibacterial activity was reported as early as the 20 th early century; in 1923, parabens were suggested as preservatives for food and pharmaceutical products; in 1932, the use of paraben as preservatives has been approved for food products and has been known for over eighty years. In 1984, nipagin ester exists in 13200 formulations of various cosmetics, and is also applied to preservation of medicines and cosmetics. It is the earliest approved synthetic preservative.
The nipagin ester is a low-toxicity high-efficiency preservative which is widely used in many aspects of food, beverage, cosmetics, medicine, feed and the like, and the annual demand of the nipagin ester in the whole country of the cosmetics industry reaches more than 50 t.
At present, the products of the parabens produced and applied in China are low-carbon chain esters, such as methyl paraben, ethyl paraben, propyl paraben and butyl paraben, and the research on long-chain paraben is less, particularly the parabens with the number of carbon atoms on an R group more than 12. Some research groups begin the research work of long-chain parabens, and make certain progress, and the emphasis is on heptylparaben and octylparaben, but the industrialization of the long-chain parabens is not realized. The reported results show that the C11 and C12 alcohol esters in the nipagin ester have very good antibacterial activity, and have very good development prospects when being used as food preservatives and feed additives.
According to the literature reports, the detection method of the nipagin dodecanoate is mainly a chemical analysis method, a potentiometric titration method, a liquid chromatography tandem mass spectrometry method and the like. The chemical analysis method and the potentiometric titration method are simple, but have long time consumption and large human error, and the liquid phase tandem mass spectrometer has high price and is rarely equipped in a common laboratory. In addition, the literature reports that the detection method of the decamethylene paraben comprises the steps of concentrating, extracting a sample and then detecting by using a high performance liquid chromatograph, and the method is time-consuming and expensive.
Therefore, the research on a simple and easy-to-operate method for detecting the dodecyl paraben is a problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a method for detecting dodecyl paraben, which solves the problems of complex operation and high price of the dodecyl paraben detection method.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for detecting lauryl paraben adopts high performance liquid chromatography to detect the content of lauryl paraben or substances containing lauryl paraben, and comprises the following steps of:
1) preparing a standard solution: preparing a plurality of parts of dodecyl paraben standard solutions according to different concentrations for later use by taking the dodecyl paraben standard product;
2) detecting a standard solution: respectively injecting all the dodecyl paraben standard solutions prepared in the step 1) into a high performance liquid chromatograph for detection to obtain chromatograms corresponding to all the dodecyl paraben standard solutions;
3) drawing a standard curve: taking the concentration of each part of the dodecyl paraben standard solution as an abscissa, and taking the peak area of a dodecyl paraben chromatographic peak in a corresponding chromatogram as an ordinate to draw a standard curve to obtain a standard curve regression equation;
4) and (3) determining the content of the sample: preparing a sample solution from a sample containing dodecyl paraben, injecting the sample solution into a high performance liquid chromatograph to detect the sample solution to obtain a sample chromatogram, and substituting the peak area of the dodecyl paraben chromatographic peak in the sample chromatogram into the standard curve regression equation in the step 3) to obtain the content of dodecyl paraben in the sample.
The technical scheme of the invention is further improved as follows: the high performance liquid chromatograph adopts a C18 reverse chromatographic column and takes 10-100% methanol water solution by volume percentage as a mobile phase.
The technical scheme of the invention is further improved as follows: the flow speed of the mobile phase is 0.6-1.0 mL/min.
The technical scheme of the invention is further improved as follows: the column temperature of the C18 reverse phase chromatographic column is 20-45 ℃.
The technical scheme of the invention is further improved as follows: detecting the dodecyl p-hydroxybenzoate standard solution injected into the high performance liquid chromatograph in the step 2) and the sample solution injected into the high performance liquid chromatograph in the step 4) by using a variable wavelength ultraviolet absorption detector.
The technical scheme of the invention is further improved as follows: the detection wavelength of the variable wavelength ultraviolet absorption detector is 245-265 nm.
The technical scheme of the invention is further improved as follows: the sample injection amount of the dodecyl paraben standard solution and the sample solution is 2-20 mu L.
The technical scheme of the invention is further improved as follows: the solvent used for preparing the lauryl paraben standard solution in the step 1) is methanol.
The technical scheme of the invention is further improved as follows: and 4) preparing the sample solution in the step 4), namely weighing the sample, putting the sample into a volumetric flask, adding methanol, ultrasonically treating to dissolve the dodecyl paraben in the sample, and diluting the methanol to a constant volume.
The technical scheme of the invention is further improved as follows: and filtering the sample solution by using a filter membrane of 0.22 mu m, and then injecting the sample solution into a high performance liquid chromatograph.
Compared with the prior art, the invention has the following progress: the method adopts a high performance liquid chromatograph to detect the dodecyl paraben, adopts an external standard method to carry out quantitative analysis, thereby determining the content of the dodecyl paraben in the sample, has high precision, high accuracy and good repeatability, can realize direct detection of the sample, greatly reduces the analysis time, is simple, easy, convenient and reliable, and reduces unnecessary complex operations such as concentration and extraction.
Furthermore, the invention adopts a C18 reverse chromatographic column and a methanol aqueous solution flowing phase to separate better.
Furthermore, the flow velocity of the mobile phase is 0.6-1.0mL/min, and in such a flow velocity range, the sample injection is carried out under the completely same conditions, so that the influence on the aspects of the separation degree, the peak shape, the symmetry degree and the like of the sample is small, the separation time is short, and the excellent separation of the dodecyl paraben sample can be realized.
Furthermore, the temperature of the C18 reverse chromatographic column is 20-45 ℃, and in such a temperature range, the sample injection is carried out under the same conditions, so that the influence on the aspects of the separation degree, the peak shape, the symmetry degree and the like of the sample is small, and the excellent separation of the dodecyl paraben sample can be realized.
Meanwhile, the invention adopts a variable wavelength ultraviolet absorption detector to detect the sample solution of the dodecyl paraben standard solution, samples are injected under the completely same conditions at the detection wavelength of 245-.
Drawings
FIG. 1 is a chromatogram of a dodecyl paraben standard solution (1000 ppm);
FIG. 2 is a chromatogram of the sample solution in example 1;
FIG. 3 is a graph of a regression equation of a standard curve in example 1;
FIG. 4 is a chromatogram of the sample solution in example 2;
FIG. 5 is a graph of a regression equation of a standard curve in example 2;
FIG. 6 is a chromatogram of the sample solution in example 3;
FIG. 7 is a graph of a regression equation of a standard curve in example 3;
FIG. 8 is a chromatogram of a feed sample solution in example 4;
FIG. 9 is a graph of a standard curve regression equation in example 4;
FIG. 10 is a chromatogram of the sample solution in example 5;
FIG. 11 is a graph of a regression equation of a standard curve in example 5;
FIG. 12 is a chromatogram of a feed sample solution of example 6;
FIG. 13 is a graph of a regression equation of a standard curve in example 6;
FIG. 14 is a chromatogram of the sample solution of example 7;
FIG. 15 is a graph of a regression equation of a standard curve in example 7;
FIG. 16 is a chromatogram of a feed sample solution of example 8;
FIG. 17 is a graph of a standard curve regression equation in example 8.
Detailed Description
The present invention is further illustrated in detail by the following specific examples, which are to be construed as merely illustrative, and not limitative of the remainder of the disclosure.
Example 1 method for detecting dodecyl paraben
The embodiment is a method for detecting dodecyl paraben, which comprises the following steps in sequence:
1) preparing a lauryl paraben standard solution:
preparing a standard stock solution: precisely weighing 1.0204g of lauryl paraben standard substance (with the purity of 98%) in a 100 mL volumetric flask, adding 60mL of methanol (analytically pure) for ultrasonic dissolution, and then using the methanol (analytically pure) for constant volume to scale to prepare 1% (10000 ppm) of lauryl paraben standard stock solution;
preparing a dodecyl paraben standard solution: accurately transferring 0.5 mL, 1.0mL, 2.0 mL, 5.0 mL, 10.0 mL and 20.0 mL of the lauryl paraben stock solution into a 100 mL volumetric flask, and respectively metering to the scale with methanol (analytically pure) to obtain the lauryl paraben standard solution A, B, C, D, E, F (wherein the concentrations of the lauryl paraben are 50 ppm, 100 ppm, 200 ppm, 500 ppm, 1000ppm and 2000 ppm respectively) for later use.
2) Detecting a standard solution:
shaking the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F uniformly, analyzing by Agilent high performance liquid chromatograph 1260 respectively, obtaining chromatogram corresponding to each dodecyl p-hydroxybenzoate standard solution, and recording peak area, wherein the liquid chromatogram of dodecyl p-hydroxybenzoate standard solution A is shown in FIG. 1. Wherein, the chromatographic conditions are as follows: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
3) Drawing a standard curve:
and (3) drawing a standard curve by taking the concentration of the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F as an abscissa and taking the peak area of a dodecyl p-hydroxybenzoate chromatographic peak in a corresponding chromatogram as an ordinate to obtain a standard curve regression equation: y =29.0865x +20.9806, R2=1, where y is the peak area of deca-hydroxybenzoate, x is the concentration of deca-hydroxybenzoate, and R is the linear correlation coefficient, see fig. 3.
4) And (3) determining the content of the sample:
preparing a sample solution:
selecting a batch of newly prepared lauryl paraben with content to be measured as a sample, precisely weighing 0.1008 g (W) lauryl paraben sample, and metering to 100 ml (V) with methanol (analytically pure)2) The volumetric flask is used for obtaining a sample stock solution. Precisely transferring four 10 ml portions of the extract (V)3) Stock solutions of samples in 50 ml (V)1) In the volumetric flask, methanol (analytically pure) solution is respectively used for constant volume to obtain a sample solution H, I, J, K;
detecting a sample solution:
after shaking the sample solution H, I, J, K uniformly, respectively using an Agilent high performance liquid chromatograph 1260 to perform sample injection analysis, simultaneously obtaining the corresponding chromatogram of each sample solution, and recording the peak area, wherein the liquid chromatogram of the sample solution H is shown in figure 2. Wherein, the chromatographic conditions are the same as those in the step 2), and specifically comprise the following steps: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
Thirdly, calculating the content of the decadiester nipagin in the sample
The calculation formula for obtaining the content of the decamethylene p-hydroxybenzoate is as follows:
in the formula: w is the percentage of the dodecyl paraben in the mass of the sample; y is the area of the peak of the dodecyl paraben measured by the sample solution; v1The volume of the sample solution is determined as the volume of ml; v2The volume of the sample stock solution is determined as the volume of ml; v3Volume of sample stock removed, ml; w is the mass of the dodecyl paraben sample, g; the specific calculation results are shown in the following table:
TABLE 1 measurement results of lauryl paraben content in sample solution
As can be seen from Table 1, the mass percent of the decamethylene paraben in this sample is about 95.19%.
Example 2 method for detecting dodecyl paraben
The embodiment is a method for detecting dodecyl paraben, which comprises the following steps in sequence:
1) preparing a lauryl paraben standard solution:
preparing a standard stock solution: precisely weighing 1.0204g of lauryl paraben standard substance (with the purity of 98%) in a 100 mL volumetric flask, adding 60mL of methanol (analytically pure) for ultrasonic dissolution, and then using the methanol (analytically pure) for constant volume to scale to prepare 1% (10000 ppm) of lauryl paraben standard stock solution;
preparing a dodecyl paraben standard solution: accurately transferring 0.5 mL, 1.0mL, 2.0 mL, 5.0 mL, 10.0 mL and 20.0 mL of the lauryl paraben stock solution into a 100 mL volumetric flask, and respectively metering to the scale with methanol (analytically pure) to obtain the lauryl paraben standard solution A, B, C, D, E, F (wherein the concentrations of the lauryl paraben are 50 ppm, 100 ppm, 200 ppm, 500 ppm, 1000ppm and 2000 ppm respectively) for later use.
2) Detecting a standard solution:
shaking the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F uniformly, respectively performing sample injection analysis by using an Agilent high performance liquid chromatograph 1260, simultaneously obtaining chromatograms corresponding to each dodecyl p-hydroxybenzoate standard solution, and recording peak areas. Wherein, the chromatographic conditions are as follows: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
3) Drawing a standard curve:
and (3) drawing a standard curve by taking the concentration of the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F as an abscissa and taking the peak area of a dodecyl p-hydroxybenzoate chromatographic peak in a corresponding chromatogram as an ordinate to obtain a standard curve regression equation: y =29.1068x-4.9274, R2=1, where y is the peak area of deca-hydroxybenzoate, x is the concentration of deca-hydroxybenzoate, and R is the linear correlation coefficient, see fig. 5.
4) And (3) determining the content of the sample:
preparing a sample solution:
selecting a batch of newly prepared lauryl paraben with content to be measured as a sample, precisely weighing 0.1011 g (W) lauryl paraben sample, and metering to 100 ml (V) with methanol (analytically pure)2) The volumetric flask is used for obtaining a sample stock solution. Precisely transferring four 10 ml portions of the extract (V)3) Stock solutions of samples in 50 ml (V)1) In the volumetric flask, methanol (analytically pure) solution is respectively used for constant volume to obtain a sample solution H, I, J, K;
detecting a sample solution:
after shaking the sample solution H, I, J, K uniformly, respectively using an Agilent high performance liquid chromatograph 1260 to perform sample injection analysis, simultaneously obtaining the corresponding chromatogram of each sample solution, and recording the peak area, wherein the liquid chromatogram of the sample solution H is shown in figure 4. Wherein, the chromatographic conditions are the same as those in the step 2), and specifically comprise the following steps: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
Thirdly, calculating the content of the decadiester nipagin in the sample
The calculation formula for obtaining the content of the decamethylene p-hydroxybenzoate is as follows:
in the formula: w is the percentage of the dodecyl paraben in the mass of the sample; y is the area of the peak of the dodecyl paraben measured by the sample solution; v1The volume of the sample solution is determined as the volume of ml; v2The volume of the sample stock solution is determined as the volume of ml; v3Volume of sample stock removed, ml; w is the mass of the dodecyl paraben sample, g; the specific calculation results are shown in the following table:
TABLE 2 measurement results of lauryl paraben content in sample solution
As can be seen from Table 2, the weight percentage of the decamethylene paraben in this sample is about 93.37%.
Example 3 method for detecting dodecyl paraben
The embodiment is a method for detecting dodecyl paraben, which comprises the following steps in sequence:
1) preparing a lauryl paraben standard solution:
preparing a standard stock solution: precisely weighing 1.0204g of lauryl paraben standard substance (with the purity of 98%) in a 100 mL volumetric flask, adding 60mL of methanol (analytically pure) for ultrasonic dissolution, and then using the methanol (analytically pure) for constant volume to scale to prepare 1% (10000 ppm) of lauryl paraben standard stock solution;
preparing a dodecyl paraben standard solution: accurately transferring 0.5 mL, 1.0mL, 2.0 mL, 5.0 mL, 10.0 mL and 20.0 mL of the lauryl paraben stock solution into a 100 mL volumetric flask, and respectively metering to the scale with methanol (analytically pure) to obtain the lauryl paraben standard solution A, B, C, D, E, F (wherein the concentrations of the lauryl paraben are 50 ppm, 100 ppm, 200 ppm, 500 ppm, 1000ppm and 2000 ppm respectively) for later use.
2) Detecting a standard solution:
shaking the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F uniformly, respectively performing sample injection analysis by using an Agilent high performance liquid chromatograph 1260, simultaneously obtaining chromatograms corresponding to each dodecyl p-hydroxybenzoate standard solution, and recording peak areas. Wherein, the chromatographic conditions are as follows: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
3) Drawing a standard curve:
and (3) drawing a standard curve by taking the concentration of the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F as an abscissa and taking the peak area of a dodecyl p-hydroxybenzoate chromatographic peak in a corresponding chromatogram as an ordinate to obtain a standard curve regression equation: y =28.6735x-37.3220, R2=1, where y is the peak area of deca-hydroxybenzoate, x is the concentration of deca-hydroxybenzoate, and R is the linear correlation coefficient, see fig. 7.
4) And (3) determining the content of the sample:
preparing a sample solution:
selecting a batch of newly prepared lauryl paraben with content to be measured as a sample, precisely weighing 0.1006 g (W) lauryl paraben sample, and metering to 100 ml (V) with methanol (analytically pure)2) ContainerAnd measuring the bottle to obtain a sample stock solution. Precisely transferring four 10 ml portions of the extract (V)3) Stock solutions of samples in 50 ml (V)1) In the volumetric flask, methanol (analytically pure) solution is respectively used for constant volume to obtain a sample solution H, I, J, K;
detecting a sample solution:
after shaking the sample solution H, I, J, K uniformly, respectively using an Agilent high performance liquid chromatograph 1260 to perform sample injection analysis, simultaneously obtaining the corresponding chromatogram of each sample solution, and recording the peak area, wherein the liquid chromatogram of the sample solution H is shown in FIG. 6. Wherein, the chromatographic conditions are the same as those in the step 2), and specifically comprise the following steps: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
Thirdly, calculating the content of the decadiester nipagin in the sample
The calculation formula for obtaining the content of the decamethylene p-hydroxybenzoate is as follows:
in the formula: w is the percentage of the dodecyl paraben in the mass of the sample; y is the area of the peak of the dodecyl paraben measured by the sample solution; v1The volume of the sample solution is determined as the volume of ml; v2The volume of the sample stock solution is determined as the volume of ml; v3Volume of sample stock removed, ml; w is the mass of the dodecyl paraben sample, g; the specific calculation results are shown in the following table:
TABLE 3 measurement results of lauryl paraben content in sample solution
As can be seen from Table 3, the weight percentage of the decamethylene paraben in this sample is about 86.32%.
Example 4 method for detecting dodecyl paraben
The embodiment is a method for detecting dodecyl paraben, which comprises the following steps in sequence:
1) preparing a lauryl paraben standard solution:
preparing a standard stock solution: precisely weighing 1.0204g of lauryl paraben standard substance (with the purity of 98%) in a 100 mL volumetric flask, adding 60mL of methanol (analytically pure) for ultrasonic dissolution, and then using the methanol (analytically pure) for constant volume to scale to prepare 1% (10000 ppm) of lauryl paraben standard stock solution;
preparing a dodecyl paraben standard solution: accurately transferring 0.5 mL, 1.0mL, 2.0 mL, 5.0 mL, 10.0 mL and 20.0 mL of the lauryl paraben stock solution into a 100 mL volumetric flask, and respectively metering to the scale with methanol (analytically pure) to obtain the lauryl paraben standard solution A, B, C, D, E, F (wherein the concentrations of the lauryl paraben are 50 ppm, 100 ppm, 200 ppm, 500 ppm, 1000ppm and 2000 ppm respectively) for later use.
2) Detecting a standard solution:
shaking the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F uniformly, respectively performing sample injection analysis by using an Agilent high performance liquid chromatograph 1260, simultaneously obtaining chromatograms corresponding to each dodecyl p-hydroxybenzoate standard solution, and recording peak areas. Wherein, the chromatographic conditions are as follows: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
3) Drawing a standard curve:
and (3) drawing a standard curve by taking the concentration of the dodecyl p-hydroxybenzoate standard solution A, B, C, D, E, F as an abscissa and taking the peak area of a dodecyl p-hydroxybenzoate chromatographic peak in a corresponding chromatogram as an ordinate to obtain a standard curve regression equation: y =29.1069x-45.9164, R2=1, where y is the peak area of deca-hydroxybenzoate, x is the concentration of deca-hydroxybenzoate, and R is the linear correlation coefficient, see fig. 9.
4) And (3) determining the content of the sample:
preparing a sample solution:
selecting a batch of feed added with dodecyl paraben as a sample, precisely weighing 10.0014 g (W) of the feed sample, placing the feed sample into a conical flask with a plug, and adding 100 ml (V)1) Obtaining sample solution by using methanol (analytically pure), and after carrying out ultrasonic treatment for 20 min, respectively marking four supernatants as sample solution H, I, J, K;
detecting a sample solution:
after shaking the sample solution H, I, J, K uniformly, respectively using an Agilent high performance liquid chromatograph 1260 to perform sample injection analysis, simultaneously obtaining the corresponding chromatogram of each sample solution, and recording the peak area, wherein the liquid chromatogram of the sample solution H is shown in figure 8. Wherein, the chromatographic conditions are the same as those in the step 2), and specifically comprise the following steps: the chromatographic column is an Agilent Pursult 5C 18 reverse chromatographic column, the length of the column is 250 mm, and the inner diameter of the column is 4.6 mu m; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 257 nm; the column temperature is 30 ℃; the mobile phase is an anhydrous methanol solution (namely a 100% methanol solution); the flow rate is 1.0 mL/min; the amount of the sample was 10. mu.L.
Thirdly, calculating the content of the decadiester nipagin in the sample
The calculation formula for obtaining the content of the decamethylene p-hydroxybenzoate is as follows:
in the formula: w is the content of the dodecyl paraben, ppm; y is the area of the peak of the dodecyl paraben measured by the sample solution; v1The volume of the sample solution is determined as the volume of ml; w is the mass of the dodecyl paraben sample, g; the specific calculation results are shown in the following table:
TABLE 4 measurement results of lauryl paraben content in sample solution
As can be seen from Table 4, the amount of decamethylene paraben in this sample was about 962.55 ppm.
Examples 5 to 8A method for detecting dodecyl p-hydroxybenzoate
Examples 5 to 8 are methods for detecting deca-hydroxybenzoate, which are the same as examples 1 to 4, but different in chromatographic conditions, as detailed in table 6:
TABLE 5 summary of different chromatographic conditions
Wherein the mobile phase methanol solution is methanol water solution, namely methanol accounts for the volume percentage of the water solution (80% methanol solution is 80% methanol and 20% water).
As can be seen from table 5, the linear regression equation obtained in example 5 is: y =28.5539x-45.0401, R2=1, see fig. 11; taking the same sample solution as example 1 for detection, and referring to fig. 10, the liquid chromatogram of one of the obtained sample solutions (the liquid chromatogram of sample solution H) is calculated from the peak area to obtain about 91.73% by mass of the dodecyl paraben;
the linear regression equation obtained in example 6 is: y =6.7237x-10.6006, R2=1, see fig. 13; taking the same sample solution as example 4 for detection, and obtaining a liquid chromatogram (liquid chromatogram of sample solution H) of one of the obtained sample solutions, referring to FIG. 12, wherein the content of the dodecyl paraben is about 944.44ppm by peak area calculation;
the linear regression equation obtained in example 7 is: y =45.5211x +2285.5693, R2=0.9944, see fig. 15; taking the same sample solution as example 1 for detection, and referring to fig. 14, the liquid chromatogram of one of the obtained sample solutions (the liquid chromatogram of sample solution H) is calculated from the peak area to obtain about 93.41% by mass of the dodecyl paraben;
the linear regression equation obtained in example 8 is: y =44.1786x-287.1630, R2=0.9999, see fig. 17; the same sample solution as in example 4 was examined, and the liquid chromatogram of one of the obtained sample solutions (the liquid chromatogram of sample solution H) was calculated from the peak area, referring to FIG. 16, to give about 951.97ppm of decamethylene paraben.
EXAMPLE 9 method Performance test
1) Precision test
Taking the dodecyl paraben standard solution A in the embodiment 1 as a subject to be investigated, shaking up, then respectively injecting samples for 6 times by using a high performance liquid chromatograph, recording peak areas, calculating a concentration value of the standard solution, and comparing the peak areas to obtain a relative standard deviation value RSD, wherein the results are shown in the following table:
table 6 precision test results (n = 6)
As can be seen from Table 6, the relative standard deviation RSD was 0.18%, and the accuracy of the detection method was high.
2) Accuracy test
The lauryl paraben standard solution B in the example 2 is taken as a subject to be investigated, the standard solution is placed at 4 ℃, sample injection is carried out at 0h, 6h, 12h, 24h, 48h and 72h respectively, peak areas are recorded, the peak areas are compared to obtain a relative standard deviation value RSD, and the results are shown in the following table.
Table 7 accuracy test results (n = 6)
As can be seen from table 7, the relative standard deviation RSD was 0.51%, the stability of the standard solution was good, and the accuracy of the detection method was high.
3) Repeatability test
The lauryl paraben standard solution C in the embodiment 3 is taken as a subject to be investigated, different testers sample the same type of instrument for 6 times at different times, peak areas are recorded, the peak areas are compared to obtain a relative standard deviation value RSD, and the result is shown in the following table.
TABLE 8 results of the repeatability tests
As can be seen from table 8, the relative standard deviation RSD was 0.93%, and the reproducibility of the detection method was good.
Claims (10)
1. A method for detecting dodecyl paraben is characterized by comprising the following steps: detecting the content of the decamethylene paraben or a substance containing the decamethylene paraben by adopting a high performance liquid chromatography, which comprises the following steps in sequence:
1) preparing a standard solution: preparing at least two parts of lauryl paraben standard solution according to different concentrations for later use by taking the lauryl paraben standard product;
2) detecting a standard solution: respectively injecting all the dodecyl paraben standard solutions prepared in the step 1) into a high performance liquid chromatograph for detection to obtain chromatograms corresponding to all the dodecyl paraben standard solutions;
3) drawing a standard curve: taking the concentration of each part of the dodecyl paraben standard solution as an abscissa, and taking the peak area of a dodecyl paraben chromatographic peak in a corresponding chromatogram as an ordinate to draw a standard curve to obtain a standard curve regression equation;
4) and (3) determining the content of the sample: preparing a sample solution by taking a sample containing the dodecyl paraben, injecting the sample solution into a high performance liquid chromatograph to detect the sample solution to obtain a sample chromatogram, substituting the peak area of the dodecyl paraben chromatographic peak in the sample chromatogram into the standard curve regression equation in the step 3), and obtaining the content of the dodecyl paraben in the sample according to an external standard method.
2. The method for detecting dodecyl paraben according to claim 1, wherein the method comprises the following steps: the high performance liquid chromatograph adopts a C18 reverse chromatographic column and takes 10-100% methanol water solution by volume percentage as a mobile phase.
3. The method for detecting dodecyl paraben according to claim 2, wherein the method comprises the following steps: the flow speed of the mobile phase is 0.6-1.0 mL/min.
4. The method for detecting dodecyl paraben according to claim 3, wherein the method comprises the following steps: the column temperature of the C18 reverse phase chromatographic column is 20-45 ℃.
5. The method for detecting dodecyl paraben according to claim 4, wherein the method comprises the following steps: detecting the dodecyl p-hydroxybenzoate standard solution injected into the high performance liquid chromatograph in the step 2) and the sample solution injected into the high performance liquid chromatograph in the step 4) by using a variable wavelength ultraviolet absorption detector.
6. The method for detecting dodecyl paraben according to claim 5, wherein the method comprises the following steps: the detection wavelength of the variable wavelength ultraviolet absorption detector is 245-265 nm.
7. The method for detecting dodecyl paraben according to claim 6, wherein the method comprises the following steps: the sample injection amount of the dodecyl paraben standard solution and the sample solution is 2-20 mu L.
8. The method for detecting dodecyl paraben according to any one of claims 1-7, wherein: the solvent used for preparing the lauryl paraben standard solution in the step 1) is methanol.
9. The method for detecting dodecyl paraben according to any one of claims 1-7, wherein: and 4) preparing the sample solution in the step 4), namely weighing the sample, putting the sample into a volumetric flask, adding methanol, ultrasonically treating to dissolve the dodecyl paraben in the sample, and diluting the methanol to a constant volume.
10. The method for detecting dodecyl paraben according to claim 9, wherein: and filtering the sample solution by using a filter membrane of 0.22 mu m, and then injecting the sample solution into a high performance liquid chromatograph.
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