CN107422050B - Method for simultaneously detecting contents of five components in pediatric humifuse euphorbia herb antidiarrheal granules - Google Patents

Method for simultaneously detecting contents of five components in pediatric humifuse euphorbia herb antidiarrheal granules Download PDF

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CN107422050B
CN107422050B CN201710303168.3A CN201710303168A CN107422050B CN 107422050 B CN107422050 B CN 107422050B CN 201710303168 A CN201710303168 A CN 201710303168A CN 107422050 B CN107422050 B CN 107422050B
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phosphoric acid
antidiarrheal
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humifuse euphorbia
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向阳
黄志军
明凯利
朱立彬
熊莉
李崇明
曾庆恢
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Jianmin Pharmaceutical Groups Corp Ltd
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Abstract

The invention discloses a method for simultaneously detecting the content of five components in pediatric humifuse euphorbia antidiarrheal particles, wherein the five components are gallic acid, baicalin, puerarin, honokiol and magnolol. The method can simultaneously detect the content of five substances in the pediatric humifuse euphorbia antidiarrheal particles, the adopted chromatographic conditions have good separation effect, short peak-producing time, good reproducibility of detection results and high accuracy, and the quality of the pediatric humifuse euphorbia antidiarrheal particles is more controllable by adopting the method.

Description

Method for simultaneously detecting contents of five components in pediatric humifuse euphorbia herb antidiarrheal granules
Technical Field
The invention relates to a content determination method of infantile humifuse euphorbia antidiarrheal granules, belonging to the field of pharmaceutical analysis.
Background
CN 102145131A discloses a Chinese medicine for treating diarrhea, which is prepared from six Chinese medicinal materials of humifuse euphorbia herb, baical skullcap root, kudzuvine root, officinal magnolia bark, Indian buead and malt, is derived from kudzuvine root, baical skullcap root and lotus root decoction in Shanghai treatise on typhoid fever, is used for treating infantile diarrhea, is currently obtained as a new medicine clinical research lot issued by the State food and drug administration, and belongs to six new Chinese medicines.
At present, the quality control of the traditional Chinese medicine is mainly realized by detecting the content of gallic acid, other components are not detected, and the quality of the product is difficult to strictly control. The applicant finds in research that the pediatric humifuse euphorbia antidiarrheal particles contain multiple components such as baicalin, puerarin, honokiol, magnolol and the like besides gallic acid, and many of the components are pharmacodynamically active components, so that if the content of the components can be strictly controlled, the quality of products can be improved, and the efficacy can be further improved.
The chemical structural formulas of the five components are as follows:
Figure BDA0001284901650000011
disclosure of Invention
The invention aims to provide a method for simultaneously detecting the contents of five components, namely gallic acid, puerarin, baicalin, honokiol and magnolol, aiming at the defect of single content determination index of children humifuse euphorbia antidiarrheal particles.
The method comprises the steps of carrying out ultrasonic extraction on a sample to be detected by using water, extracting an extracting solution by using a nonpolar organic solvent, and then detecting the extracting solution by using a high performance liquid chromatograph, wherein the high performance liquid chromatograph contains an ultraviolet detector, the set detection wavelength of the ultraviolet detector is 250-280 nm, a chromatographic column of the high performance liquid chromatograph is a C18 chromatographic column, a mobile phase is a mixed solution of 0.1-0.5% phosphoric acid water solution and 0.1-1% cyclohexane, gradient elution is adopted, the column temperature is 25-35 ℃, and the number of theoretical plates is not less than 5000 according to the gallic acid peak.
The pediatric humifuse euphorbia antidiarrheal granules are disclosed in the patent document CN 102145131A and are prepared from the following Chinese medicinal materials in parts by weight:
20-50 parts of humifuse euphorbia herb, 6-18 parts of scutellaria baicalensis, 6-18 parts of kudzu root
5-12 parts of magnolia officinalis, 5-12 parts of poria cocos, and 5-12 parts of malt.
Preferably, the non-polar organic solvent is chloroform.
Preferably, the set detection wavelength of the ultraviolet detector is 260 nm.
Preferably, the mobile phase is a mixture of 0.1% phosphoric acid in water and 0.1% cyclohexane in methanol.
Preferably, in the gradient elution, the volume ratio of the phosphoric acid aqueous solution in each time period and the mobile phase is: 0-5 min, and 90% of phosphoric acid aqueous solution; 5-15 min, and 90-82% of phosphoric acid aqueous solution; 15-30 min, and 82-68% of phosphoric acid aqueous solution; 30-37 min, and 68-59% of phosphoric acid aqueous solution; 37-50 min, and 59-20% of phosphoric acid aqueous solution; 50-62 min, 20% phosphoric acid water solution.
Preferably, the column temperature is 28 ℃.
The invention has the beneficial effects that: the method provided by the invention can be used for simultaneously detecting the content of five substances in the infantile humifuse euphorbia antidiarrheal particles, and has the advantages of high detection efficiency, high speed, low cost, good separation effect of the adopted chromatographic conditions, short peak-producing time, good reproducibility of the detection result and high accuracy. The method can control the quality of the infantile diarrhea-relieving granule.
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FIG. 1 is a high performance liquid chromatogram obtained by extraction with 70% ethanol in the investigation of the sample preparation method.
FIG. 2 is a high performance liquid chromatogram obtained by extraction with chloroform from water during investigation of the sample preparation method.
FIG. 3 is a high performance liquid chromatogram obtained using a detection wavelength of 250 nm.
FIG. 4 is a high performance liquid chromatogram obtained using a detection wavelength of 260 nm.
FIG. 5 is a high performance liquid chromatogram obtained using a detection wavelength of 271 nm.
FIG. 6 is a high performance liquid chromatogram obtained with mobile phase A being 0.5% phosphoric acid aqueous solution and mobile phase B being methanol.
FIG. 7 is a high performance liquid chromatogram obtained with mobile phase A being 0.1% phosphoric acid aqueous solution and mobile phase B being methanol.
FIG. 8 is a high performance liquid chromatogram obtained when mobile phase A was a 0.1% phosphoric acid aqueous solution and mobile phase B was methanol (containing 0.1% cyclohexane).
FIG. 9 is a high performance liquid chromatogram obtained when mobile phase A was a 0.1% phosphoric acid aqueous solution and mobile phase B was methanol (containing 1% cyclohexane).
FIG. 10 is a high performance liquid chromatogram obtained under the mobile phase gradient elution condition (1) in example 4.
FIG. 11 is a high performance liquid chromatogram obtained under the mobile phase gradient elution condition (2) in example 4.
FIG. 12 is a high performance liquid chromatogram obtained under the mobile phase gradient elution condition (3) in example 4.
FIG. 13 is a high performance liquid chromatogram at a column temperature of 28 ℃.
FIG. 14 is a high performance liquid chromatogram at a column temperature of 35 ℃.
Detailed Description
The present invention will be described in detail below with reference to examples. The pediatric humifuse euphorbia antidiarrheal granules in each example were prepared according to example 1 in CN 102145131 a and provided by the member pharmaceutical industry group ltd.
EXAMPLE 1 selection of sample preparation methods
The preparation method of the sample solution comprises the following steps: 1. taking the products with different filling amounts, mixing uniformly, taking a proper amount, grinding, taking about 1.5g, precisely weighing, placing in a 50ml conical flask with a plug, precisely adding 50ml of 70% (weight concentration) ethanol, sealing the plug, weighing, ultrasonically treating (power 250W, frequency 33kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% ethanol, shaking uniformly, filtering, precisely taking 10ml of continuous filtrate in a 25ml measuring flask, and fixing the volume with methanol to obtain the product.
2. Taking the product under the condition of different filling amount, mixing uniformly, taking a proper amount, grinding, taking about 1.5g, precisely weighing, placing in a 50ml conical flask with a plug, precisely adding 50ml of water, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W, frequency 33kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with water, shaking up, filtering, precisely taking 10ml of subsequent filtrate, extracting with chloroform for three times, 20ml each time, removing a chloroform layer, transferring a water layer to a 25ml measuring flask, and fixing the volume with methanol to obtain the product.
The instrument comprises the following steps: agilent1260 type high performance liquid chromatograph series (Agilent technologies, USA, including quaternary pump, autosampler, column oven, ultraviolet detector, M8301AA chromatography workstation)
Mobile phase: 0.1% by weight of aqueous phosphoric acid as mobile phase A: methanol solution containing 0.1% by weight of cyclohexane as mobile phase B
Gradient elution conditions:
Figure BDA0001284901650000041
column temperature: 28 ℃; detection wavelength: 260 nm; sample introduction amount: 10ul of
As a result: as shown in FIG. 1 and FIG. 2, the extraction with chloroform from water is preferred because it can significantly reduce impurities, such as 46min, 47min, and 7min, better target peaks, compared with 70% ethanol extraction.
EXAMPLE 2 selection of wavelength
Preparation of a sample solution: taking the product under the condition of different filling amount, mixing uniformly, taking a proper amount, grinding, taking about 1.5g, precisely weighing, placing in a 50ml conical flask with a plug, precisely adding 50ml of water, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W, frequency 33kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with water, shaking up, filtering, precisely taking 10ml of subsequent filtrate, extracting with chloroform for three times, 20ml each time, removing a chloroform layer, transferring a water layer to a 25ml measuring flask, and fixing the volume with methanol to obtain the product.
Detection wavelength: 250nm, 260nm and 271nm
Other conditions were the same as in example 1.
As a result: as can be seen from fig. 3, 4, and 5, the baseline shift is significant at a wavelength of 250 nm; at a wavelength of 260nm, the peak response of each substance is larger than that of 271nm (in the isobologram, the color of the peak of each substance at 260nm is darker than that of the peak at 271nm, indicating that the absorption is stronger), and the number of the peaks of each substance displayed is 2 more than that of the peak at 271nm, so that 260nm is the most suitable detection wavelength.
EXAMPLE 3 selection of Mobile phase
(1) A is 0.5% phosphoric acid aqueous solution: b is methanol
(2) A is 0.1% phosphoric acid aqueous solution: b is methanol
(3) A is 0.1% phosphoric acid aqueous solution: b is methanol (containing 0.1% cyclohexane)
(4) A is 0.1% phosphoric acid aqueous solution: b is methanol (containing 1% cyclohexane)
Detection wavelength: 260nm
Other conditions were the same as in example 1.
As a result: as can be seen from FIGS. 6 to 9, the chromatographic peak at 26min in FIG. 6 has a poor separation effect and is not completely separated; the separation is not complete at 29min and 43min in FIG. 7. In fig. 9, the mobile phase is completely unsuitable, and the substances cannot be separated. In FIG. 8, the peak pattern and the degree of separation are best when 0.1% phosphoric acid solution and methanol (containing 0.1% cyclohexane) are used as mobile phases.
Example 4 selection of conditions for mobile phase gradient elution
Mobile phase: 0.1% phosphoric acid aqueous solution as mobile phase a: methanol (containing 0.1% cyclohexane) as mobile phase B
Column temperature: 28 ℃; detection wavelength: 260 nm; sample introduction amount: 10ul of
Gradient elution conditions:
Figure BDA0001284901650000051
Figure BDA0001284901650000061
(2)
Figure BDA0001284901650000062
(3)
Figure BDA0001284901650000063
as a result: as shown in fig. 10-12, in fig. 11, the peak-off time is too fast, and the target peaks at 7min, 15min and 29min are not completely separated; in FIG. 12, the peak pattern at 26min was not good, and it could not be judged whether the separation was complete, and FIG. 10 was good, so that the gradient elution condition was selected (1).
EXAMPLE 5 selection of column temperature
Mobile phase: 0.1% phosphoric acid aqueous solution as mobile phase a: methanol (containing 0.1% cyclohexane) as mobile phase B
Column temperature: 28 ℃ and 35 DEG C
Other conditions were the same as in example 1.
As a result: as shown in fig. 13 and 14, the column temperature was 35 ℃, the peak-out time was somewhat shortened, and at 42min, the separation effect became worse; further, as compared with FIG. 13, the column temperature is increased and the number of peaks is increased, for example, at 54min, and therefore, 28 ℃ is preferable.
Example 6 method verification
1. Positioning and system adaptability test of five substances
(1) Test method
Preparation of a test solution: taking the product under the condition of different filling amount, mixing uniformly, taking a proper amount, grinding, taking about 1.5g, precisely weighing, placing in a 50ml conical flask with a plug, precisely adding 50ml of water, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W, frequency 33kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with water, shaking up, filtering, precisely taking 10ml of subsequent filtrate, extracting with chloroform for three times, 20ml each time, removing a chloroform layer, transferring a water layer to a 25ml measuring flask, and fixing the volume with methanol to obtain the product.
The instrument comprises the following steps: agilent1260 type high performance liquid chromatograph series (Agilent technologies, USA, including quaternary pump, autosampler, column oven, ultraviolet detector, M8301AA chromatography workstation)
Mobile phase: 0.1% phosphoric acid aqueous solution as mobile phase a: methanol (containing 0.1% cyclohexane) as mobile phase B;
gradient elution conditions:
Figure BDA0001284901650000071
column temperature: 28 deg.C
Detection wavelength: 260nm
Sample introduction amount: 10ul of
(2) The calculation method comprises the following steps:
Figure BDA0001284901650000081
Ci pairsThe concentration (mg/ml) of each specific substance as a control solution
Ai pairsPeak area for each specific substance control solution
ASample iPeak area for each specific substance
WSample (A)Weighing the sample (g)
(3) Analytical method validation
Preparing a reference substance solution: accurately weighing appropriate amount of standard substances of gallic acid, puerarin, baicalin, honokiol, and magnolol, and making into mixed solution containing gallic acid, puerarin, baicalin, honokiol, and magnolol 15ug, 60ug, 40ug, 13ug, and 20ug, respectively per 1 ml.
The preparation and determination method of the test solution comprises the following steps: the sample preparation method and the sample injection determination under the liquid chromatography condition established in the above embodiment are carried out.
The results are shown in Table 1.
TABLE 1 positioning and system adaptability test result table of five substances
Name of substance Corresponding peak Retention time Relative retention time Degree of separation
Gallic acid 1 peak 7.377 - 5.89
Puerarin and its preparation method 3 peak of 28.967 0.18 1.87
Baicalin 9 peak 42.365 0.31 1.26
Honokiol 18 peak 51.867 0.42 3.72
Magnolol 19 peak (1) 53.344 0.53 2.91
2. Linearity
The study was conducted by taking 6 concentration points in the range from the quantitative limit concentration to the index concentration of not higher than 150%. The linear relationship is plotted as a function of the measured response signal (peak area) versus analyte concentration, and a linear regression is performed using the least squares method, with the correlation coefficient R2The linear regression coefficient R is required to confirm a good linear relationship2Should be not less than 0.990, the results are shown in Table 2.
TABLE 2 Standard curves, correlation coefficients and correction factors for the five substances
Name of substance Standard curve Correlation coefficient Correction factor
Gallic acid Y＝3.0261x-0.7541 R2＝0.9992 0.91
Puerarin and its preparation method Y＝3.8704x+0.0891 R2＝0.9986 0.78
Baicalin Y＝4.5051x-2.7588 R2＝0.9996 0.96
Honokiol Y＝6.7253x-3.8956 R2＝0.9981 1.00
Magnolol Y＝5.8965x-4.0967 R2＝0.9987 0.95
3. Repeatability of
6 sample solutions with the same concentration are prepared and tested, wherein 1 needle is injected into each solution, the relative standard deviation of 6 content measurement results is required to be not more than 2.0%, and the results are shown in a table 3.
TABLE 3 repeatability test results for the five substance assay
Sample (I) Gallic acid Puerarin and its preparation method Baicalin Honokiol Magnolol
RSD 1.32％ 1.21％ 1.98％ 1.83％ 1.47％
The results show that: the RSD value of each component is in a required range, which shows that the repeatability result of the detection method is good.
4. Accuracy of
Recovery, expressed as a percentage, was calculated by adding known amounts of each component and measuring the ratio of the measured results to the theoretical values for the known components in the sample, requiring recovery between 95.0% and 105.0%, and the results are shown in table 4.
TABLE 4 results of recovery measurement of five substances
Sample (I) Gallic acid Puerarin and its preparation method Baicalin Honokiol Magnolol
Average recovery rate 98.51％ 99.42％ 97.72％ 99.01％ 100.24％
The results show that: the method has good accuracy in measuring each substance.
Example 7 sample determination
(1) Preparation of a test solution: taking the infantile humifuse euphorbia antidiarrheal particles with different loading amounts, uniformly mixing, taking a proper amount, grinding, taking about 1.5g, precisely weighing, placing in a 50ml conical flask with a plug, precisely adding 50ml of water, sealing the plug, weighing, carrying out ultrasonic treatment (power of 250W and frequency of 33kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with water, shaking uniformly, filtering, precisely taking 10ml of subsequent filtrate, extracting with chloroform for three times, 20ml each time, removing a chloroform layer, transferring a water layer to a 25ml measuring flask, and fixing the volume with methanol to obtain the infantile humifuse euphorbia antidiarrheal preparation.
(2) Preparation of control solutions: accurately weighing appropriate amount of standard substances of gallic acid, puerarin, baicalin, honokiol, and magnolol, and making into mixed solution containing gallic acid, puerarin, baicalin, honokiol, and magnolol 15ug, 60ug, 40ug, 13ug, and 20ug, respectively per 1 ml.
(3) Chromatographic conditions and system adaptability: the instrument comprises the following steps: agilent1260 type high performance liquid chromatograph series (Agilent technologies, USA, including quaternary pump, autosampler, column oven, ultraviolet detector, M8301AA chromatography workstation)
Mobile phase: 0.1% phosphoric acid aqueous solution (a): methanol (containing 0.1% cyclohexane) (B)
Gradient elution conditions:
Figure BDA0001284901650000101
column temperature: 28 deg.C
Detection wavelength: 260nm
Sample introduction amount: 10ul of
(4) And (3) determination: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and measuring.
(5) Calculating the formula: see (2) in example 6.
(6) As a result: the contents of the respective substances measured are shown in Table 5.
TABLE 56 content of five substances in the sample lots
Batches of Gallic acid Puerarin and its preparation method Baicalin Magnolol Honokiol
160701 0.253％ 0.421％ 0.884％ 0.017％ 0.008％
160301 0.255％ 0.402％ 0.871％ 0.016％ 0.007％
150902 0.262％ 0.413％ 0.910％ 0.013％ 0.004％
150901 0.266％ 0.444％ 0.908％ 0.010％ 0.006％
150601 0.255％ 0.462％ 0.895％ 0.013％ 0.005％
150201 0.267％ 0.453％ 0.878％ 0.009％ 0.006％

Claims (2)

1. A method for simultaneously detecting the content of five components in an infantile humifuse euphorbia antidiarrheal granule is disclosed, wherein the infantile humifuse euphorbia antidiarrheal granule is prepared from the following Chinese medicinal materials in parts by weight:
Figure FDA0002360544970000011
the method is characterized in that: the five components are gallic acid, baicalin, puerarin, honokiol and magnolol, the method comprises the steps of carrying out ultrasonic extraction on a sample to be detected by using water, extracting an extracting solution by using chloroform, and then detecting by using a high performance liquid chromatograph, wherein the high performance liquid chromatograph contains an ultraviolet detector, the set detection wavelength of the ultraviolet detector is 260nm, a chromatographic column of the high performance liquid chromatograph is a C18 chromatographic column, a mobile phase is a mixed solution of 0.1% phosphoric acid water solution and 0.1% cyclohexane methanol solution, gradient elution is adopted, the column temperature is 25-35 ℃, the number of theoretical plates is not less than 5000 according to the peak of the gallic acid,
in the gradient elution, the volume ratio of the 0.1% phosphoric acid aqueous solution in each time period and the mobile phase is respectively as follows: 0-5 min, 90% of 0.1% phosphoric acid aqueous solution; 5-15 min, 90 → 82% of 0.1% phosphoric acid water solution; 15-30 min, 82 → 68% of 0.1% phosphoric acid water solution; 30-37 min, 68 → 59% of 0.1% phosphoric acid water solution; 37-50 min, 59 → 20% of 0.1% phosphoric acid water solution; 50-62 min, 20% of 0.1% phosphoric acid water solution.
2. The method for simultaneously detecting the content of five components in the infantile humifuse euphorbia antidiarrheal particles as claimed in claim 1, wherein the method comprises the following steps: the column temperature was 28 ℃.
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