CN112986478B - Determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets - Google Patents
Determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets Download PDFInfo
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Abstract
The invention provides a determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets, which comprises the following steps: (1) preparing a test solution: taking 10 compound liquorice tablets, precisely weighing, grinding, precisely weighing about 1 tablet, putting into a 50mL measuring flask, adding an appropriate amount of diluent, performing ultrasonic treatment, cooling, diluting with the diluent to scale, shaking up, filtering with a 0.45 μm microporous membrane, and taking the subsequent filtrate as a sample solution; (2) preparation of a reference solution: weighing sodium benzoate, potassium sorbate (calculated as sorbic acid), methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate standard, adding diluent, dissolving, and making into reference solutions with different concentrations; (3) and (4) measuring by using a reversed-phase high performance liquid chromatography. The method realizes content determination of sodium benzoate in compound radix Glycyrrhizae tablet, and can be used for screening and quantitative analysis of whether sorbic acid and hydroxyphenyl preservative are illegally added.
Description
Technical Field
The invention relates to the technical field of drug detection, in particular to a detection method for screening and quantitatively analyzing preservative components in compound liquorice tablets.
Background
The compound liquorice tablet is a compound preparation with good cough relieving and phlegm eliminating effects. The quality standard is recorded in the second part of 2020 edition of Chinese pharmacopoeia, and the prescription comprises licorice extract powder, opium powder or poppy fruit extract powder, star anise oil, camphor, sodium benzoate and the like. Modern pharmacological studies show that the licorice extract is a protective cough-relieving expectorant, the poppy fruit extract powder has a strong cough-relieving effect, and the star anise oil and camphor have strong volatility, can stimulate the smooth muscle of the respiratory tract, promote the discharge of sputum and play a role in reducing phlegm; sodium benzoate is used as antiseptic.
The compound liquorice tablet mainly comprises liquorice extractum, is sweet in taste and easy to absorb moisture, and is extremely easy to be polluted by microorganisms in the production and use processes, so that a certain amount of sodium benzoate is added in the prescription to achieve the bacteriostatic effect. The common preservatives in the pharmaceutical preparations include sorbic acid, hydroxybenzoates and the like in addition to benzoic acid; the excessive use of the preservative can cause certain harm to the metabolism of human viscera. The Chinese pharmacopoeia also makes clear requirements on the dosage, and stipulates that the dosage of sorbic acid and benzoic acid is not more than 0.3 percent, and the dosage of hydroxyphenyl ester is not more than 0.05 percent; however, the pharmacopoeia standards do not load the relevant detection methods. For the quality control of the compound liquorice tablets, the existing standard only takes glycyrrhizic acid and morphine as main materials, and the content determination method and limit requirements of sodium benzoate are not carried; in the reported literature, a method for screening and detecting the preservative component in the compound liquorice tablets is not found. Therefore, the comprehensive control cannot be realized on whether the preservative components are illegally and excessively added or are added beyond the standard in the preparation production process.
In the prior art, although a detection method aiming at preservative components in different preparations exists, the components of the compound liquorice tablets are complex and are easily interfered by each component in the detection process, and the extraction mode, the detection condition and the like of the existing method are not suitable for detecting each preservative component in the compound liquorice tablet preparation. For example, the Huangke et al disclose a method for simultaneously measuring methylparaben, propylparaben and dibutylhydroxytoluene in a gel (CN 104374843B); adopting Agilent ZORBAX SB-C184.6mm multiplied by 250mm and 5 mu m is taken as a chromatographic column, acetonitrile-1% acetic acid water solution is taken as a mobile phase for gradient elution, and dual wavelengths (Pr-PHBA, Me-PHBA detection wavelength is 250nm-260nm, BHT detection wavelength is 270nm-286nm) are adopted for analysis and detection. The results of the detection of the compound liquorice tablets by using the method show that chromatographic peaks of all components in a test sample can not be well separated from preservative components such as sodium benzoate, sorbic acid and the like, and the separation degree can not meet the analysis requirements.
In order to more comprehensively control the quality of the compound liquorice tablets and prevent excessive or illegal addition of preservative components in the preparation production process, a proper detection method is established for determining the content of sodium benzoate in the compound liquorice tablets and screening whether other preservative components are illegally added or not, so that the compound liquorice tablets have very important significance.
Disclosure of Invention
In order to solve the problem that a detection method aiming at the preservative in the compound liquorice tablets is lacked in the prior art, the invention provides a reversed-phase liquid-phase high-performance chromatography for screening and quantitatively analyzing the preservative components in the compound liquorice tablets, which not only realizes the content determination of sodium benzoate in the compound liquorice tablet prescription, but also can screen and quantitatively analyze whether sorbic acid and hydroxybenzene ester preservatives are illegally added.
The invention provides a determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets, which comprises the following steps:
1. preparing a test solution: taking 10 compound liquorice tablets, precisely weighing, grinding, precisely weighing 0.15g (each tablet weighs about 0.15 g), putting into a 50mL measuring flask, adding 20-30 mL of diluent, performing ultrasonic treatment, cooling, diluting to scale with the diluent, shaking up, filtering through a 0.45 mu m microporous membrane, and taking the subsequent filtrate as a test solution.
2. The preparation of the reference solution comprises the following specific steps:
1) weighing appropriate amount of sodium benzoate and potassium sorbate (calculated as sorbic acid) as reference, dissolving in diluent, and quantitatively diluting to obtain sodium benzoate and sorbic acid of about 4.0 mg/mL-1The solution of (4) for use;
2) accurately weighing appropriate amount of methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate, respectively dissolving in diluent, quantitatively diluting, and making into tablet containing methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate about 0.5 mg/mL-1The solution of (4) for use;
3) precisely measuring 5mL of the reference solutions, placing in a 50mL measuring flask, diluting to scale with diluent, shaking, and storing as reference stock solution.
4) Precisely measuring the reference stock solutions 0.2mL, 0.5mL, 1.0mL, 2.5mL, 5mL and 8mL respectively, placing in 10mL measuring bottles, diluting to scale with diluent, shaking up, and making into reference solutions with different concentrations.
3. And (3) reverse phase high performance liquid chromatography determination:
the HPLC chromatographic conditions were as follows:
a chromatographic column: c18A chromatographic column; mobile phase: acetonitrile (A) -0.1% formic acid 0.02 mol. L-1Potassium dihydrogen phosphate (B); gradient elution; the flow rate was 1.0 mL/min-1(ii) a A detector: a diode array detector; detection wavelength: detecting double wavelengths; sample introduction amount: 10 μ L.
Preferably, the diluent in step 1 is a mixed solution prepared from ethanol, water and glacial acetic acid according to a volume ratio of 45:50: 5.
Preferably, the ultrasonic time in step 1 is 30 minutes, and the ultrasonic power is 1500W.
Preferably, C is as described in step 318The chromatographic column is Shim-pack GIST C18The chromatographic column with the column specification of 4.6mm multiplied by 250mm and the particle size of 5 mu m can ensure that chromatographic peaks of all components in a reference substance and a test solution can achieve good separation effect.
Preferably, the gradient elution described in step 3 comprises the following steps: 0min, 96% B; 10min, 90% B; 25min, 65% B; 35min, 45% B; 40min, 35% B; 60min, 35% B; 61min, 96% B; 71min, 96% B.
Preferably, the chromatographic conditions in step 3 are 35 ℃ at the column temperature.
Preferably, the detection wavelength in step 3 is: the dual wavelength detection is 254nm (methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate, butyl hydroxybenzoate) and 240nm (sodium benzoate and sorbic acid).
Has the advantages that:
the invention provides a determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets, which takes ethanol-water-glacial acetic acid (45: 50: 5) solution as an extraction solvent of the compound liquorice tablets, adopts reversed phase high performance liquid chromatography and uses C18The chromatographic column is an analytical column, and acetonitrile-0.1% formic acid is 0.02 mol.L-1Performing gradient elution with potassium dihydrogen phosphate as mobile phase, and performing dual-wavelength detection (254 nm, 240 nm); the content determination of sodium benzoate in the compound liquorice tablet prescription is realized, and simultaneously, the screening and quantitative analysis can be carried out on whether other preservatives such as sorbic acid, methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate, butyl hydroxybenzoate and the like are illegally added.
In the development of the method, the selection of an extraction solvent and a mobile phase system and the setting of gradient elution play a crucial role in the accuracy and specificity of the method. Through multiple experiments, the inventor respectively compares the extraction effects of different solvents, and repeatedly screens and optimizes chromatographic conditions and an elution program, finally overcomes the defects of poor solvent extraction effect, interference of each component on measured components and other factors, obtains a method which has strong specificity, high sensitivity and simple operation, is suitable for screening and quantitative analysis of each preservative component in compound liquorice tablets, and provides a method basis for more comprehensively evaluating the quality of the compound liquorice tablets and controlling the use of the preservative.
Drawings
FIG. 1 is an HPLC chromatogram of a control (254 nm), wherein 1. sodium benzoate; 2. sorbic acid; 3. methyl paraben; 4. glycyrrhizic acid; 5. ethylparaben; propyl hydroxybenzoate;
FIG. 2 is an HPLC chromatogram of a control (240 nm);
FIG. 3 is an HPLC chromatogram of a test sample (254 nm);
FIG. 4 is an HPLC chromatogram of a test sample (240 nm);
FIG. 5 is an HPLC chromatogram of a negative sample (254 nm);
FIG. 6 is an HPLC chromatogram of a negative sample (240 nm).
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Instrument and reagent
Agilent1260 ii high performance liquid chromatograph (prep quaternary pump, online degasser, DAD detector, autosampler, Open LAB CDS 2.X chemical workstation), XS205DU electronic analytical balance (Mettler Toledo corporation), ultrasound.
Methanol, acetonitrile, ethanol and formic acid are used as chromatographic purities, potassium dihydrogen phosphate is used as analytical purities, and water is ultrapure water. Sodium benzoate (100433-. The compound liquorice tablets are from 6 batches of 3 different manufacturers.
Second, analysis method
1. Preparation of the Diluent
Weighing appropriate amounts of ethanol, water and glacial acetic acid, and preparing a mixed solution with a volume ratio of ethanol-water-glacial acetic acid of 45:50:5 for later use.
2. Preparation of test solution
Taking 10 compound liquorice tablets, precisely weighing, grinding, precisely weighing 0.1532g (average tablet weight is 0.1502 g), placing in a 50mL measuring flask, adding 25mL of diluent, performing ultrasonic treatment for 30min at ultrasonic power of 1500W, cooling, diluting with the diluent to scale, shaking up, filtering through a 0.45 mu m microporous membrane, and taking the subsequent filtrate as a test solution.
2. Preparation of control solutions
1) Weighing appropriate amount of sodium benzoate and potassium sorbate (calculated as sorbic acid) as reference, dissolving in diluent, and quantitatively diluting to obtain sodium benzoate and sorbic acid of about 4.0 mg/mL-1The solution of (4) for use;
2) accurately weighing appropriate amount of methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate, respectively dissolving in diluent, quantitatively diluting, and making into tablet containing methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate about 0.5 mg/mL-1The solution of (4) for use;
3) precisely measuring 5mL of the reference solutions obtained in the steps 1) and 2), placing in a 50mL measuring flask, diluting with diluent to scale, shaking, and storing as reference stock solution.
4) Precisely measuring the reference stock solutions 0.2mL, 0.5mL, 1.0mL, 2.5mL, 5mL and 8mL respectively, placing in 10mL measuring bottles, diluting to scale with diluent, shaking up, and making into reference solutions with different concentrations.
3. Preparation of negative sample solution
Preparing a negative sample without adding sodium benzoate according to the formula proportion of the compound liquorice tablets, and preparing according to the method in the step 1 to obtain a negative sample solution.
4. Chromatographic conditions and System suitability test
The Agilent1260 II high performance liquid chromatography system adopts diode arrayColumn detector, column Shim GIST C18Chromatographic column (4.6 mm × 250mm, 5 μm) with mobile phase of 0.02 mol.L of acetonitrile-0.1% formic acid-1Potassium dihydrogen phosphate, gradient elution conditions are shown in Table 1, flow rate is 1.0 mL/min-1Column temperature 35 ℃, sample injection: 10 μ L, and detecting wavelength of 254nm (methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate, butyl hydroxybenzoate) and 240nm (sodium benzoate and sorbic acid). Under the chromatographic conditions, the control solution is measured, the theoretical plate number of each component chromatographic peak is more than 3000, good baseline separation is realized, the separation degree is more than 1.5, and the tailing factors meet the requirements (see figure 1).
TABLE 1 gradient elution procedure
5. Linear range, detection limit and quantification limit tests
The control solutions were precisely pipetted at 10. mu.L each, and the measurement was carried out under the above-mentioned chromatographic conditions. Concentration (mg. mL) using the peak area of each compound as the ordinate-1) Linear regression was performed for the abscissa to obtain a standard curve.
Sorbic acid and hydroxyphenyl ester compounds are used as illegal addition components outside a prescription to screen target objects, and the detection limit and the quantitative limit of the sorbic acid and hydroxyphenyl ester compounds are further explained. The negative samples were taken as a blank matrix and added at a low concentration level, diluted stepwise and subjected to sample injection measurement, and the detection Limit (LOD) was calculated with a signal-to-noise ratio (S/N) of 3 and the quantification Limit (LOQ) was calculated with a signal-to-noise ratio (S/N) of 10, and the results are shown in Table 2.
Table 2: linear relationship of each component and detection limit and quantitative limit
6. Precision test
Precisely sucking 10 μ L of the same reference solution, continuously repeating sample injection for 6 times according to the above chromatographic conditions, and calculating peak area of each compound. As a result, the RSDs of the peak areas of sodium benzoate, sorbic acid, methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate were 1.3%, 0.9%, 1.2%, 1.4% and 1.5%, respectively.
7. Recovery test
Precisely weighing 6 parts (containing 0.21 mg/tablet of sodium benzoate and no other preservatives) of a sample with a known content, precisely weighing about 0.5 tablet of each part, precisely adding 2mL of a reference stock solution into a 50mL volumetric flask, and calculating the recovery rate according to the chromatographic conditions as described above, thus obtaining: the sample recovery rates (n = 6) of sodium benzoate, sorbic acid, methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate are respectively 99.6%, 95.8%, 99.6%, 98.9%, 100.5% and 98.4%; RSD is 2.0%, 1.2%, 2.3%, 2.0%, 1.9%, respectively.
8. Stability test
The same recovery test solution was allowed to stand at room temperature, and the RSD of the peak areas of sodium benzoate, sorbic acid, methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate was determined to be 1.5%, 1.7%, 1.2%, 1.8%, 2.0% and 1.5% for 0, 2, 4, 8, 12 and 24 hours, respectively.
9. Sample assay
Taking 6 batches of compound liquorice tablet samples from 3 different manufacturers, preparing 3 parts of parallel test sample solutions for each batch of samples according to the step 2, analyzing and screening 6 preservative components according to the chromatographic conditions, wherein sorbic acid, methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate in the 6 batches of samples are not detected, so that the phenomenon that the preservatives are illegally added and used in the 6 batches of products of the 3 manufacturers is avoided, and the content of sodium benzoate is calculated by an external standard method, and the result is shown in table 3.
Table 3 results of sample analysis (mg/tablet) (n = 3)
Example two: investigation of extraction effect of different solvents on positive sample
1. Preparation of Positive samples
According to the prescription proportion of the compound liquorice tablets, certain amounts of potassium sorbate (calculated according to sorbic acid), methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate are respectively added to prepare positive samples (containing sodium benzoate, potassium sorbate (calculated according to sorbic acid), methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate, which are respectively 2.02 mg/tablet, 0.45 mg/tablet, 0.075 mg/tablet, 0.076 mg/tablet, 0.074 mg/tablet and 0.075 mg/tablet) with known preservative amounts.
2. The other conditions are the same as the first example, and the extraction effects of different solvent diluents on positive samples are respectively examined, and the results are shown in tables 4.1-4.4.
TABLE 4.1 methanol extraction Effect
TABLE 4.2 ethanol extraction Effect
TABLE 4.3 ethanol-Water (1: 1) extraction Effect
TABLE 4.4 extraction Effect of ethanol-water-glacial acetic acid (45: 50: 5)
The result shows that the best extraction effect is achieved by using ethanol-water-glacial acetic acid (45: 50: 5) as an extraction solvent.
Example three: selection of detection wavelength in chromatographic conditions
Other conditions are the same as the first embodiment, the control solution is subjected to chromatographic analysis, a DAD detector is adopted to obtain the ultraviolet absorption spectrum of each compound, wherein the maximum absorption wavelength of benzoic acid is 224nm, sorbic acid, methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate have the maximum absorption at the wavelength of 254nm, the interference of each component of the compound liquorice tablet and the detection sensitivity of an object to be detected are comprehensively considered, and finally, the detection wavelengths of methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate are 254nm, and the detection wavelengths of sodium benzoate and sorbic acid are 240 nm.
Example four: investigation of different mobile phase compositions
Other conditions are the same as in the first example, methanol is respectively selected to be 0.02 mol.L-1Potassium dihydrogen phosphate solution, acetonitrile-water, acetonitrile-0.02 mol.L-1Potassium dihydrogen phosphate solution and acetonitrile-0.1% formic acid 0.02 mol.L-1The potassium dihydrogen phosphate solution system is used as a mobile phase, and the influence of different mobile phases on the chromatographic separation of each component is examined.
The results show that the appearance order of glycyrrhizic acid in the compound liquorice tablets is closer to that of benzoic acid and sorbic acid, the three components in the first three mobile phase systems can not meet the separation requirement, and the glycyrrhizic acid in acetonitrile-0.02 mol.L-1After a certain amount of formic acid is added into the potassium dihydrogen phosphate solution, the separation effect is obviously improved; the separation degrees among benzoic acid, sorbic acid and glycyrrhizic acid all meet the analysis requirement; finally, the mobile phase system is determined to be 0.02 mol.L of acetonitrile-0.1 percent formic acid-1Potassium dihydrogen phosphate solution.
Example five: selection of mobile phase composition ratio in gradient leaching procedure
Other conditions were the same as in example one, and gradient elution was performed as shown in Table 5; as a result, the hydroxyphenyl ester component in the test solution is interfered by adjacent impurity peaks, and the resolution does not meet the analysis requirement.
TABLE 5 gradient elution procedure
Claims (3)
1. A determination method for screening and quantitatively analyzing preservative components in compound liquorice tablets is characterized by comprising the following steps:
(1) preparing a test solution: taking 10 compound liquorice tablets, precisely weighing, grinding, precisely weighing 0.15g, placing in a 50mL measuring flask, adding 25mL of diluent, performing ultrasonic treatment, cooling, diluting to scale with the diluent, shaking up, filtering with a 0.45-micrometer microporous membrane, and taking a subsequent filtrate as a sample solution, wherein the diluent is a mixed solution prepared from ethanol, water and glacial acetic acid according to a volume ratio of 45:50: 5;
(2) preparation of a reference solution: weighing sodium benzoate, potassium sorbate, methyl hydroxybenzoate, ethylparaben, propyl hydroxybenzoate and butyl hydroxybenzoate standard, adding diluent, dissolving, and making into reference solutions with different concentrations, wherein potassium sorbate is calculated by sorbic acid;
(3) reversed phase high performance liquid chromatography, wherein the chromatographic column is Shim-pack GIST C18A chromatographic column with the specification of 4.6mm multiplied by 250mm, the particle size of 5 mu m and the column temperature of 35 ℃; mobile phase: a is acetonitrile, B is 0.02 mol.L of 0.1% formic acid-1Potassium dihydrogen phosphate; gradient elution: the flow rate was 1.0 mL/min-1(ii) a A detector: a diode array detector; detection wavelength: detecting double wavelengths; sample introduction amount: 10 mu L of the solution;
the gradient elution steps are as follows: 0min, 96% B; 10min, 90% B; 25min, 65% B; 35min, 45% B; 40min, 35% B; 60min, 35% B; 61min, 96% B; 71min, 96% B.
2. The assay method for screening and quantitatively analyzing the preservative component in the compound licorice tablet according to claim 1, wherein the dual wavelength detection of step (3): the detection wavelength of methyl hydroxybenzoate, ethyl hydroxybenzoate, propyl hydroxybenzoate and butyl hydroxybenzoate is 254nm, and the detection wavelength of sodium benzoate and sorbic acid is 240 nm.
3. The assay method for screening and quantitatively analyzing the preservative component in the compound licorice tablets according to claim 1, wherein the ultrasonic time in step (1) is 30 minutes, and the ultrasonic power is 1500W.
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