CN113791143A - Quality control method of angelica dahurica in wind-dispelling pain-relieving capsule - Google Patents

Quality control method of angelica dahurica in wind-dispelling pain-relieving capsule Download PDF

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CN113791143A
CN113791143A CN202110853155.XA CN202110853155A CN113791143A CN 113791143 A CN113791143 A CN 113791143A CN 202110853155 A CN202110853155 A CN 202110853155A CN 113791143 A CN113791143 A CN 113791143A
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张小利
穆竟伟
袁元
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SHANGHAI KAIBAO PHARMACEUTICAL CO Ltd
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention relates to a quality control method of angelica dahurica in a wind-dispelling pain-relieving capsule, which comprises the following steps: identification according to thin layer chromatography: whether fluorescent spots of the same color appear in the thin-layer chromatography of the first test solution at positions corresponding to the thin-layer chromatography of the first control solution and the thin-layer chromatography of the second control solution; according to the high performance liquid chromatography: based on the total amount of imperatorin and isoimperatorin, the content of radix Angelicae Dahuricae in each 0.29g sample is less than 0.30 mg. The quality control method establishes a corresponding method for qualitatively and quantitatively detecting the angelica dahurica in the wind-dispelling pain-relieving capsule, and has better linear relation, parallelism, repeatability, accuracy, stability, intermediate precision, specificity and durability, thereby establishing the quality standard specification of the angelica dahurica in the wind-dispelling pain-relieving capsule.

Description

Quality control method of angelica dahurica in wind-dispelling pain-relieving capsule
Technical Field
The invention relates to the technical field of pharmaceutical analysis, in particular to a quality control method of radix angelicae in a wind-dispelling and pain-relieving capsule.
Background
The capsule for dispelling wind and relieving pain is a prescription prepared by combining clinical experience on the basis of 'Jiefao Tang' in dialectical records, and the dahurian angelica root is a ministerial medicine component in the capsule.
The radix Angelicae Dahuricae is a perennial big herb with a height of 1-2.5 m, a cylindrical root, a stem base with a diameter of 2-5 cm, a basal leaf with a pinnate division, a multiple umbrella-shaped inflorescence with terminal or lateral growth, and a long fruit with a shape of oval to oval. The main varieties include radix Angelicae Dahuricae, and radix Angelicae Dahuricae (original variety). The root is used as a medicine and has the functions of dispelling diseases, removing dampness, expelling pus, promoting granulation, promoting blood circulation, relieving pain and the like. Can be used for treating wind-cold type common cold, headache, rhinitis, and toothache. It can also be used as perfume for treating leucorrhea with red and white discharge, pain, furuncle, and toxic swelling. Some northern provinces are cultivated, so that the cultivation is carried out by self production and self sale, and the cultivation is carried out by only a few provinces. Typically under the forest, at the forest edge, beside the stream, in shrubs and on the valley grassland.
The contents of the wind-dispelling pain-relieving capsule are slightly bitter and pungent in taste, can activate blood circulation to dispel wind, warm meridians to relieve pain, and are commonly used for treating the symptoms of migraine, such as migraine with congealing cold and blood stasis, i.e. symptoms of over-normal headache or parietal headache with dwarf and urgent pain, reduced heat, no thirst, hot drink preference, clear and long urine, loose and thin stool, pale and dark or purple tongue, white and moist fur, and slow or tense pulse. However, the wind-dispelling pain-relieving capsule lacks of comprehensive and normative methodology research data at present, and no normative quality standard is established for angelica dahurica.
Therefore, a quality control method of angelica dahurica in the wind-dispelling pain-relieving capsule is urgently needed.
Disclosure of Invention
The invention aims to provide a quality control method of angelica dahurica in a wind-dispelling and pain-relieving capsule aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
provides a quality control method of angelica dahurica in the wind-dispelling pain-relieving capsule, which comprises the following steps:
s1, grinding the sample, adding a first solvent, heating and refluxing, cooling, filtering, volatilizing the filtrate, adding a second solvent into the residue, and dissolving to obtain a first test solution; adding radix Angelicae Dahuricae control medicinal material into first solvent, heating and refluxing, cooling, filtering, volatilizing filtrate, adding second solvent into residue, and dissolving to obtain first control solution; identification according to thin layer chromatography: whether fluorescent spots with the same color appear in the thin-layer chromatography of the first test solution at the positions corresponding to the thin-layer chromatography of the first control solution and the thin-layer chromatography of the second control solution;
s2, mixing and grinding the sample, precisely weighing, precisely adding a third solvent, weighing, performing ultrasonic treatment, taking out, cooling, weighing again, complementing the reduced weight with the third solvent, shaking up, filtering, and taking a subsequent filtrate to obtain a second sample solution; according to the high performance liquid chromatography: based on the total amount of imperatorin and isoimperatorin, the content of radix Angelicae Dahuricae in each 0.29g sample is less than 0.30 mg.
Preferably, the first solvent is diethyl ether; the second solvent is ethyl acetate; the third solvent is methanol.
Preferably, the thin layer chromatography comprises: and sucking the first sample solution, the first reference substance solution and the second reference substance solution, respectively dropping on the same thin-layer plate, unfolding, taking out, drying in the air, and placing under an ultraviolet lamp for inspection.
Preferably, said second control solution is prepared by adding 0.5mg of imperatorin control and 0.5mg of isoimperatorin control per 1mL of said second solvent.
Preferably, the conditions of the thin layer chromatography include: the sample amount is 5 muL; the thin layer plate is a silica gel G plate; the developing solvent is toluene-ethyl acetate; the wavelength of the ultraviolet lamp is 365 nm.
Preferably, the volume ratio of toluene to ethyl acetate in the developing solvent is 10: 1.
Preferably, the high performance liquid chromatography comprises: and precisely sucking the second sample solution and the third reference solution, and respectively injecting into a high performance liquid chromatograph.
Preferably, the third control solution is prepared by adding 100 μ g of precisely-weighed imperatorin control and 30 μ g of precisely-weighed isoimperatorin control to 1mL of the third solvent.
Preferably, the conditions of the high performance liquid chromatography include: the sample injection amount is 10 mu L; the filler is octadecylsilane chemically bonded silica; the mobile phase is acetonitrile-water; the detection wavelength is 250 nm; the number of theoretical plates is not less than 6000 calculated according to imperatorin peak.
Preferably, the volume ratio between acetonitrile and water in the mobile phase is 60: 40.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the quality control method establishes a corresponding method for qualitatively and quantitatively detecting the angelica dahurica in the wind-dispelling pain-relieving capsule, and has better linear relation, parallelism, repeatability, accuracy, stability, intermediate precision, specificity and durability, thereby establishing the quality standard specification of the angelica dahurica in the wind-dispelling pain-relieving capsule.
Drawings
FIG. 1 is a thin layer chromatogram (room temperature, medium humidity) for identifying radix Angelicae Dahuricae;
wherein Lane 1 is imperatorin reference solution; lane 2 is isoimperatorin reference solution; lane 3 is a test solution of a blank sample (lacking radix angelicae); lane 4 is radix Angelicae Dahuricae reference medicinal solution; lane 5 is the second sample solution (lot No. S141201); lane 6 is the second test solution (lot No. S141202); lane 7 is the second test solution (lot No. S141203);
FIG. 2 is a liquid chromatogram of radix Angelicae Dahuricae in the capsule for dispelling pathogenic wind and relieving pain;
wherein, the picture A is a liquid chromatogram of the second test sample solution; fig. B is a liquid chromatogram of a mixed solution of an imperatorin control and an isoimperatorin control (the chromatographic peaks are imperatorin and isoimperatorin from left to right in order); and the figure C is a liquid chromatogram of a blank sample (lacking the radix angelicae dahuricae) solution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
Example 1
The embodiment provides a quality control method of angelica dahurica in a wind-dispelling pain-relieving capsule, which comprises the following steps:
s1, grinding 4g of sample, adding 80mL of diethyl ether, heating and refluxing for 40min, cooling, filtering, volatilizing the filtrate, and adding 1mL of ethyl acetate into the residue to dissolve to obtain a first test solution; adding 40mL of diethyl ether into 1g of radix Angelicae Dahuricae control medicinal material, heating and refluxing, cooling, filtering, volatilizing filtrate, and adding 1mL of ethyl acetate into residue to dissolve to obtain first control solution; adding ethyl acetate into imperatorin reference substance and isoimperatorin reference substance to obtain second reference substance solution with concentration of 0.5 mg/mL; according to the test of thin layer chromatography (appendix VI B of the 2010 version of Chinese pharmacopoeia), sucking 5 μ L of each of the first test solution, the first control solution and the second control solution, respectively dropping the solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate (10:1) as a developing agent, taking out, drying in the air, and placing under an ultraviolet lamp (365nm) for inspection: whether fluorescent spots with the same color appear in the thin-layer chromatography of the first test solution at the positions corresponding to the thin-layer chromatography of the first control solution and the thin-layer chromatography of the second control solution;
s2, mixing and grinding the samples, precisely weighing 1.0g, placing the sample in a conical flask with a plug, precisely adding 25mL of methanol, weighing, carrying out ultrasonic treatment (power is 300W and frequency is 45kHz) for 30min, taking out, cooling, weighing again, complementing the weight loss by methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a second sample solution; precisely weighing imperatorin reference substance and isoimperatorin reference substance, and adding methanol to obtain a third reference substance solution with imperatorin concentration of 100 μ g/mL and isoimperatorin concentration of 30 μ g/mL; according to the high performance liquid chromatography (appendix VI D of the first part of the 2010 edition of the Chinese pharmacopoeia), precisely absorbing 10 mu L of each of the second test solution and the third reference solution, respectively injecting into a high performance liquid chromatograph (a filler is octadecylsilane chemically bonded silica; a mobile phase is acetonitrile-water (60: 40); a detection wavelength is 250 nm; the number of theoretical plates is not less than 6000 calculated according to the imperatorin peak), and determining: with imperatorin (C)16H14O4) And isoimperatorin (C)16H14O4) Whether the content of the angelica dahurica in each sample (namely 0.29g) is less than 0.30mg or not is determined.
Example 2: examination of thin layer chromatography
(1) Examination of extraction method
According to the investigation, when the method comprises the steps of taking 4g of a sample, grinding the sample, adding 80mL of diethyl ether, heating and refluxing for 40min, cooling, filtering, volatilizing the filtrate, and adding 1mL of ethyl acetate into residues to dissolve the residues to obtain a first test solution, the characteristic spots of the radix angelicae in the thin-layer chromatography of the first test solution are clear.
(2) Investigation of amount of dots
According to investigation, when the sampling amount of the angelica dahurica reference medicinal material is 1g, the concentrations of the imperatorin reference substance and the isoimperatorin reference substance solution are all 0.5mg/mL, and the sample application amounts of the first sample solution, the angelica dahurica reference medicinal material solution, the imperatorin reference substance solution and the isoimperatorin reference substance solution are all 5 muL, the size of spots on the thin-layer chromatography is moderate.
(3) Examination of developing Agents
Examining more than ten developing agents such as petroleum ether (30-60 ℃) -ethyl ether (3:2), petroleum ether (30-60 ℃) -ethyl ether (2:1), petroleum ether (30-60 ℃) -ethyl ether (1:1), petroleum ether (30-60 ℃) -ethyl acetate (1:1), toluene-ethyl acetate (8:2), petroleum ether (30-60 ℃) -ethyl acetate (85:15), petroleum ether (30-60 ℃) -ethyl acetate (9:1), toluene-ethyl acetate (15:1), cyclohexane-ethyl acetate (17:3), toluene-ethyl acetate (10:1), toluene-ethyl acetate (7:1), and the like, and if toluene-ethyl acetate (10:1) is used as the developing agent, a silica gel G thin layer plate, an ultraviolet lamp (365nm) is used for inspection and the like, the first test solution has good thin-layer chromatography separation degree, fluorescent spots with the same color are shown at the positions corresponding to the thin-layer chromatography of the angelica dahurica reference medicinal material solution, the thin-layer chromatography of the imperatorin reference solution and the thin-layer chromatography of the isoimperatorin reference solution, and the thin-layer chromatography of the test solution of the blank sample (lacking the angelica dahurica) has no interference.
(4) Investigation of specificity
After the test solution of the blank sample (lacking radix angelicae) is prepared by the same method, the thin-layer chromatography of the test solution of the blank sample (lacking radix angelicae) does not show main fluorescent spots with the same color at the position corresponding to the thin-layer chromatography of the radix angelicae contrast medicinal material solution, and the fluorescent spots with the same color do not show at the position corresponding to the thin-layer chromatography of the imperatorin contrast solution and the thin-layer chromatography of the isoimperatorin contrast solution, so that the method has no interference on radix angelicae identification and has good specificity (see figure 1).
(5) Investigation of durability of the method
By adopting the identification method, the conditions of different sources (imported and domestic prefabricated silica gel G thin-layer plates), different temperatures (room temperature, namely 20 ℃ and low temperature, namely 4 ℃), different humidities (low humidity, namely RH is 32 percent and high humidity, namely RH is 88 percent) and the like of the thin-layer plate are considered, and the results are satisfactory development and separation, which shows that the durability of the invention is better under different conditions.
Example 3: examination of high Performance liquid chromatography
(1) Investigation of chromatographic columns
3 chromatographic columns of different manufacturers, brands and lengths are investigated, which comprises: agilent ZORBAX eclipse XDB-C18 (Agilent, 5 μm, 4.6X 150mm), Phenomenex Luna (Philomena, 5 μm C18(2)100A, 5 μm, 4.6X 250mm), and Agilent ZORBAX SB-C18 (Agilent, 5 μm, 4.6X 250 mm). The result shows that chromatographic columns with different specifications have better response and separation to imperatorin and isoimperatorin in the invention, and the method has better durability.
(2) Selection of mobile phase
Looking at methanol-water (55:45) as the mobile phase, we found that imperatorin separated poorly;
other mobile phase conditions are considered, and when acetonitrile-water (60:40) is used as the mobile phase, the separation degree of the component to be detected and adjacent chromatographic peaks is better, so that the component to be detected is selected.
(3) Selection of detection wavelength
Diode array scanning is carried out on chromatographic peaks of imperatorin and isoimperatorin, and it is found that when the absorption wavelength is 250nm, the response values of two components to be detected are high, so that the detection wavelength is selected to be 250nm finally.
(4) Investigation of Linear relationships
Precisely sucking 1 muL and 2 muL of mixed reference solution (the concentration of imperatorin is 0.10325mg/mL, the concentration of imperatorin is 0.0305274mg/mL) and 1 muL, 2 muL, 5 muL, 10 muL and 20 muL of mixed reference solution (the concentration of imperatorin is 0.413mg/mL, the concentration of imperatorin is 0.1221096mg/mL) respectively, injecting into a liquid chromatograph, drawing a standard curve by taking the sample injection amount as a horizontal coordinate and the peak area as a vertical coordinate, and calculating a regression equation. The relationship between the concentration and the amount of sample is shown in tables 1 and 2.
TABLE 1 relationship between imperatorin concentration and sample size (n 7)
Concentration (mg/mL) Sample volume (μ L) Sample volume (ug) Peak area
0.10325 1 0.10325 487.75241
0.10325 2 0.2065 949.67413
0.413 1 0.413 1909.80994
0.413 2 0.826 3822.25391
0.413 5 2.065 9477.4209
0.413 10 4.13 18200
0.413 20 8.26 33871.5
The linear equation is: y is 4113.89682X +411.51929, and the regression coefficients are: and r is 0.9992. The measurement result shows that the imperatorin sample amount is in the range of 0.10325-8.26 mug, and the sample amount and the peak area have good linear relation.
TABLE 2 relationship between Isoimperatorin concentration and sample size (n 7)
Figure BDA0003183102340000061
Figure BDA0003183102340000071
The linear equation is: y is 3755.99028X +0.21730, and the regression coefficients are: r is 1.0000. The measurement result shows that the sample amount of isoimperatorin is in the range of 0.0305274-2.442192 mug, and the sample amount and the peak area have good linear relation.
(5) Control solution parallelism test
Precisely sucking 10 μ L of mixed control solution (imperatorin concentration is 0.10325mg/mL, imperatorin concentration is 0.0305274mg/mL), continuously feeding for 6 times, respectively, and measuring peak areas of imperatorin and isoimperatorin, the results are shown in Table 3.
Table 3 results of the parallelism test of the control solutions (n ═ 6)
Numbering Peak area (imperatorin) Peak area (Isoimperatorin)
1 4759.50098 1144.96484
2 4760.89160 1146.00403
3 4761.63770 1145.82654
4 4764.93750 1145.87817
5 4766.13428 1147.07788
6 4768.80225 1146.69043
Average 4763.65072 1146.07365
RSD(％) 0.07 0.06
From the above table, it is clear that RSD of the peak areas of imperatorin and isoimperatorin obtained by 6 consecutive analyses are both small, and the parallelism of the control solution is good.
(6) Ultrasound time investigation
The ultrasonic time was 15 minutes, 30 minutes, 60 minutes, 90 minutes and 120 minutes, and the results of the imperatorin measurement were 2.37mg/g, 2.40mg/g, 2.39mg/g, 2.40mg/g and 2.39mg/g, respectively, and the results of the isoimperatorin measurement were 0.72mg/g, 0.73mg/g and 0.73mg/g, respectively. When the sonication time was 30 minutes, the extraction was more complete, so a sonication time of 30 minutes was chosen.
(7) Repeatability survey
Samples of 1.0g powder were taken in 6 replicates and processed as described above for the test solution preparation, and the results are shown in tables 4 and 5.
Table 4 imperatorin reproducibility test (n ═ 6)
Figure BDA0003183102340000081
Table 5 isoimperatorin reproducibility test (n ═ 6)
Figure BDA0003183102340000082
As can be seen from the table, the relative standard deviation of the repeatability measurement results of imperatorin and isoimperatorin of 6 samples is less than 1%, and the method has good repeatability.
(8) Accuracy survey
0.5g of sample powder was sampled in 9 copies and precisely weighed, and 2.5mL, 3.0mL and 3.5mL (3 copies each) of mixed control solutions (imperatorin concentration of 0.413mg/mL and isoimperatorin concentration of 0.1221096mg/mL) were precisely added as low-concentration, medium-concentration and high-concentration samples, respectively, and the samples were treated according to the above-mentioned test solution preparation method to calculate the sample recovery rates, and the results are shown in Table 6 and Table 7.
Table 6 imperatorin accuracy test results (n ═ 9)
Figure BDA0003183102340000091
Table 7 isoimperatorin accuracy test results (n ═ 9)
Figure BDA0003183102340000092
From the above results, the accuracy of the mapping method is better.
(9) Stability testing of test solutions
The sample solution was sampled and analyzed at 0 hour, 1 hour, 2 hours, 4 hours, 6 hours, 9 hours, 12 hours, 15 hours, 18 hours, 21 hours, and 24 hours, and the peak areas were recorded, and the results are shown in Table 8.
TABLE 8 stability results for test solutions
Figure BDA0003183102340000093
Figure BDA0003183102340000101
The above test results show that imperatorin and isoimperatorin in the test solution are substantially stable within 24 hours.
(10) Intermediate precision investigation
In order to examine the influence of random variation factors on precision, the content of 3 batches of samples was determined by different analysts on different dates and different instruments according to the proposed method, and the results are shown in table 9.
TABLE 9 results of intermediate precision measurement (unit: mg/granule)
Figure BDA0003183102340000102
The results show that the measurement results of different analysts on different dates, different instruments and different chromatographic columns are basically consistent, and the intermediate precision of the method is good.
(11) Specialization inspection
A blank sample (without radix angelicae dahuricae) is taken and determined according to a drawn method, and the result shows that the blank sample solution has no interference at the chromatographic peaks of imperatorin and isoimperatorin and has good specificity (see figure 2).
In conclusion, the quality control method of the invention establishes a corresponding method for qualitative and quantitative detection of the angelica dahurica in the wind-dispelling pain-relieving capsule, and has better linear relation, parallelism, repeatability, accuracy, stability, intermediate precision, specificity and durability, thereby formulating the quality standard specification of the angelica dahurica in the wind-dispelling pain-relieving capsule.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

Claims (10)

1. A quality control method of radix angelicae in a wind-dispelling and pain-relieving capsule is characterized by comprising the following steps:
s1, grinding the sample, adding a first solvent, heating and refluxing, cooling, filtering, volatilizing the filtrate, adding a second solvent into the residue, and dissolving to obtain a first test solution; adding radix Angelicae Dahuricae control medicinal material into first solvent, heating and refluxing, cooling, filtering, volatilizing filtrate, adding second solvent into residue, and dissolving to obtain first control solution; identification according to thin layer chromatography: whether fluorescent spots with the same color appear in the thin-layer chromatography of the first test solution at the positions corresponding to the thin-layer chromatography of the first control solution and the thin-layer chromatography of the second control solution;
s2, mixing and grinding the sample, precisely weighing, precisely adding a third solvent, weighing, performing ultrasonic treatment, taking out, cooling, weighing again, complementing the reduced weight with the third solvent, shaking up, filtering, and taking a subsequent filtrate to obtain a second sample solution; according to the high performance liquid chromatography: based on the total amount of imperatorin and isoimperatorin, the content of radix Angelicae Dahuricae in each 0.29g sample is less than 0.30 mg.
2. The quality control method according to claim 1, wherein the first solvent is diethyl ether; the second solvent is ethyl acetate; the third solvent is methanol.
3. The quality control method according to claim 1, wherein the thin layer chromatography comprises: and sucking the first sample solution, the first reference substance solution and the second reference substance solution, respectively dropping on the same thin-layer plate, unfolding, taking out, drying in the air, and placing under an ultraviolet lamp for inspection.
4. The quality control method according to claim 3, wherein the second control solution is prepared by adding 0.5mg of imperatorin control and 0.5mg of isoimperatorin control per 1mL of the second solvent.
5. The quality control method according to claim 3, wherein the conditions of the thin layer chromatography include: the sample amount is 5 muL; the thin layer plate is a silica gel G plate; the developing solvent is toluene-ethyl acetate; the wavelength of the ultraviolet lamp is 365 nm.
6. The quality control method according to claim 5, wherein the volume ratio of toluene to ethyl acetate in the developing solvent is 10: 1.
7. The quality control method according to claim 1, wherein the high performance liquid chromatography comprises: and precisely sucking the second sample solution and the third reference solution, and respectively injecting into a high performance liquid chromatograph.
8. The quality control method according to claim 7, wherein the third control solution is prepared by adding 100 μ g of precisely-weighed imperatorin control and 30 μ g of precisely-weighed isoimperatorin control to 1mL of the third solvent.
9. The quality control method according to claim 7, wherein the conditions of the high performance liquid chromatography include: the sample injection amount is 10 mu L; the filler is octadecylsilane chemically bonded silica; the mobile phase is acetonitrile-water; the detection wavelength is 250 nm; the number of theoretical plates is not less than 6000 calculated according to imperatorin peak.
10. The quality control method according to claim 9, wherein the volume ratio of acetonitrile to water in the mobile phase is 60: 40.
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Application publication date: 20211214