CN111999415B - HPLC fingerprint spectrum establishment method for purple light tablet - Google Patents

HPLC fingerprint spectrum establishment method for purple light tablet Download PDF

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CN111999415B
CN111999415B CN202010876262.XA CN202010876262A CN111999415B CN 111999415 B CN111999415 B CN 111999415B CN 202010876262 A CN202010876262 A CN 202010876262A CN 111999415 B CN111999415 B CN 111999415B
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purple light
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ginsenoside
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夏淑英
旷春兰
肖绍川
康爱华
贾天亮
刘厚权
刘鹏飞
张金良
张小梅
康兴东
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JIANGXI PUZHENG PHARMACEUTICAL CO Ltd
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
    • G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components

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Abstract

The invention discloses a method for establishing a purple light tablet fingerprint and the fingerprint thereof, wherein the method comprises the following steps: step 1, preparing a sample solution; step 2, preparing a reference substance solution; step 3 chromatographic conditions: ODS C 18 (4.6 mm. Times.250 mm,5 μm) column; mobile phase a is acetonitrile; mobile phase B is aqueous solution; the detection wavelength is 203nm; column temperature: 20 ℃; flow rate: 1.0ml . min ‑1 The method comprises the steps of carrying out a first treatment on the surface of the And step 4, measuring to obtain the fingerprint spectrum of the purple light tablet. The invention also carries out methodological verification on the establishment method of the fingerprint spectrum. The fingerprint spectrum of the purple light sheet, which is measured by the method, has the advantages of high precision, good stability, good repeatability and high similarity, can effectively control the quality of the purple light sheet, ensures the uniformity and stability of the quality of the product, and further ensures the safety and effectiveness of the product.

Description

HPLC fingerprint spectrum establishment method for purple light tablet
Technical Field
The invention relates to a quality control method of a traditional Chinese medicine preparation, in particular to a method for establishing a purple light tablet preparation fingerprint by using a high performance liquid chromatography and the purple light tablet fingerprint obtained by the method.
Background
The Zilamp tablet is prepared from herba Erigerontis, saviae Miltiorrhizae radix, notoginseng radix, radix Puerariae and Glycyrrhrizae radix, wherein Notoginseng radix is dried root and rhizome of Notoginseng radix Panax notonginseng (Burk.) F.H.Chen of Araliaceae, and is collected in Chinese pharmacopoeia standard. The main active ingredients are ginsenoside compounds such as ginsenoside Rg1, ginsenoside Rb1 and the like, and have pharmacological effects of removing blood stasis, stopping bleeding, detumescence, relieving pain and the like. The Zi lamp tablet has effects of warming channels, dispelling cold, invigorating qi, promoting blood circulation, relieving spasm and pain, and can be used for treating cervical spondylosis.
The traditional Chinese medicine fingerprint is a spectrogram or a chromatogram which can characterize the characteristics of traditional Chinese medicine or Chinese patent medicine by applying modern analysis and test technology from the perspective of the traditional Chinese medicine quality basis. The traditional Chinese medicine fingerprint can comprehensively reflect the types and the amounts of the internal chemical components contained in the traditional Chinese medicine, so as to reflect the quality of the traditional Chinese medicine, and particularly the effective components of the traditional Chinese medicine are mostly undefined at the present stage, and the traditional Chinese medicine quality is effectively characterized by adopting the traditional Chinese medicine fingerprint mode. The advantages of the traditional Chinese medicine fingerprint in the aspect of overall quality control of traditional Chinese medicines are widely accepted by people in the industry, and the quality control of the plant medicines is carried out by adopting the fingerprint in the world.
The fingerprint of the purple light piece is established, and the method has important significance for quality control of the purple light piece, improvement of quality standard of the purple light piece and medication safety.
At present, the quality of the purple light tablet is controlled by a fingerprint spectrum, which is not reported in the literature.
Disclosure of Invention
The invention aims to provide a method for establishing HPLC fingerprint of a purple light tablet. The method comprises the steps of preparing the purple light slice into a sample solution, and analyzing and detecting the purple light slice by using a high performance liquid chromatography to obtain an HPLC fingerprint of the purple light slice, thereby providing a powerful support basis for the intrinsic quality evaluation of the purple light slice.
The invention provides a method for establishing HPLC fingerprint of a purple light slice, which comprises the following steps:
step 1, preparing a sample solution: precisely weighing 1g of the content of the purple lamp slice, placing the purple lamp slice into a conical bottle with a plug, precisely adding 25-50 ml of water-saturated n-butanol, weighing, carrying out reflux extraction for 2-3 hours, taking out, cooling, supplementing the reduced weight with the water-saturated n-butanol, filtering, precisely weighing 15-25 ml of a subsequent filtrate, placing the filtrate into a separating funnel, washing with ammonia test solution for 2 times, each time 25ml, discarding the ammonia test solution, evaporating the n-butanol solution to dryness, dissolving residues with methanol, concentrating to 10-15 ml, filtering with a microporous filter membrane, and obtaining a sample solution;
step 2, preparing a reference substance solution: taking 5-15 mg of ginsenoside Rg1 and ginsenoside Rb1 reference substances respectively, placing into 50ml volumetric flasks, adding methanol to a certain volume to scale, shaking uniformly, filtering with microporous membrane, and collecting the subsequent filtrate to obtain reference substance solution;
step 3, chromatographic conditions: ODS C 18 Chromatographic column (4.6 mm. Times.250 mm,5 μm); the mobile phase A is acetonitrile, the mobile phase B is aqueous solution, and gradient elution is carried out; the detection wavelength is 203nm; column temperature: 10-30 ℃; flow rate: 1.0 ml/min -1 The method comprises the steps of carrying out a first treatment on the surface of the Sample injection amount: 10 μl;
the volume ratio concentration of the gradient elution program of the method is as follows:
elution time ratio of mobile phase A to mobile phase B
0min 10％ 90％
15min 19％ 81％
30min 33％ 67％
40min 35％ 65％
50min 37％ 63％
65min 38％ 62％
Step 4, measuring: and precisely sucking 10-20 mu l of the sample solution, injecting into a liquid chromatograph, and measuring by high performance liquid chromatography to obtain the fingerprint of the purple light tablet.
In the step 1 of the invention, the preparation of the ultraviolet lamp chip test sample solution comprises the following steps: precisely weighing 1g of the content of the purple lamp slice, placing the purple lamp slice into a conical bottle with a plug, precisely adding 50ml of water-saturated n-butanol, weighing, reflux-extracting for 2 hours, taking out, cooling, supplementing the reduced weight with the water-saturated n-butanol, filtering, precisely weighing 25ml of continuous filtrate, placing into a separating funnel, washing for 2 times with ammonia test solution, each 25ml of the ammonia test solution, discarding the ammonia test solution, evaporating the n-butanol solution, dissolving residues in methanol, concentrating to 10ml, filtering with a microporous filter membrane, and taking the continuous filtrate to obtain a sample solution;
preparation of the control solution in step 2 of the invention: taking 10mg of ginsenoside Rg1 reference substance and 7.5mg of ginsenoside Rb1 reference substance, respectively placing into 50ml volumetric flasks, adding methanol to constant volume to scale, shaking, filtering with microporous membrane, and collecting the subsequent filtrate to obtain reference substance solution;
chromatographic conditions in step 3 of the invention: ODS C 18 (4.6 mm. Times.250 mm,5 μm) column; mobile phase a is acetonitrile; the mobile phase B is aqueous solution, and gradient elution is carried out, and the procedure is as follows: 0 min-15 min,90% B is reduced to 81% B,10% A is increased to 19% A; the detection wavelength is 203nm; column temperature: 20 ℃; flow rate: 1.0 ml/min -1 . The elution procedure is a gradient elution procedure.
The determination in the step 4 of the invention is as follows: and precisely sucking 10 mu l of the sample solution, injecting into a liquid chromatograph, and measuring by using a high performance liquid chromatography to obtain the fingerprint of the purple light slice.
Compared with the prior art, the invention has the beneficial effects that:
the similarity of the fingerprint spectrum of the purple light sheet established by the method is more than 0.90, the product quality can be effectively represented, and the quality of the product can be monitored more conveniently.
The invention adopts the high-efficiency liquid phase to establish the standard fingerprint, controls the quality of the product and the medicinal materials through multiple index components, can more effectively ensure the long-term stability of the quality of the product, and further ensures the safety and the effectiveness of the curative effect.
The invention has the advantages of rapidness, stability, high precision, strong repeatability, wide application range and the like, and is beneficial to the omnibearing control of the quality stability of the ultraviolet lamp sheet.
Drawings
FIG. 1 is a fingerprint spectrum comparison spectrum of the purple light tablet;
FIG. 2 is a fingerprint of the batch of purple light patches;
FIG. 3 purple light patch peak assignment;
Detailed Description
Example 1: purple light tablet fingerprint control method
Instrument: agilent 1260 high performance liquid chromatograph; ultraviolet detector
Reagent: ginsenoside Rg1 reference (batch number: 110703-201731), ginsenoside Rb1 reference (batch number: 110704-201827) are from Chinese food and drug assay institute; the mobile phase acetonitrile is chromatographic purity, water is ultrapure water, and the rest reagents are analytical purity.
Sample solution preparation: precisely weighing 1g of the content of the purple lamp slice, placing the purple lamp slice into a conical bottle with a plug, precisely adding 50ml of water-saturated n-butanol, weighing, reflux-extracting for 2 hours, taking out, cooling, supplementing the reduced weight with the water-saturated n-butanol, filtering, precisely weighing 25ml of continuous filtrate, placing into a separating funnel, washing for 2 times with ammonia test solution, each 25ml of the ammonia test solution, discarding the ammonia test solution, evaporating the n-butanol solution, dissolving residues in methanol, concentrating to 10ml, filtering with a microporous filter membrane, and taking the continuous filtrate to obtain a sample solution;
preparing a reference substance solution: taking 10mg of ginsenoside Rg1 reference substance and 7.5mg of ginsenoside Rb1 reference substance, respectively placing into 50ml volumetric flasks, adding methanol to constant volume to scale, shaking, filtering with microporous membrane, and collecting the subsequent filtrate to obtain reference substance solution;
chromatographic conditions: ODS C 18 (4.6 mm. Times.250 mm,5 μm) column; mobile phase a is acetonitrile; mobile phase B is aqueous solution; the detection wavelength is 203nm; column temperature: 20 ℃; flow rate: 1.0 ml/min -1 ；
The volume ratio concentration of the gradient elution program is as follows:
Figure BDA0002649835210000031
Figure BDA0002649835210000041
and (3) measuring: and precisely sucking 10 mu l of the sample solution, injecting into a liquid chromatograph, and measuring by using a high performance liquid chromatography to obtain the fingerprint of the purple light slice.
The fingerprint of the purple light tablet established by the method of the embodiment 1 has 11 characteristic shared peaks, wherein the No. 1 peak is erigeron breviscapus, red sage root and kudzuvine root shared peaks, the No. 2 peak is erigeron breviscapus special peak, the No. 3 peak and the No. 4 peak are erigeron breviscapus, red sage root, notoginseng, kudzuvine root and licorice shared peaks, the No. 5 peak is notoginseng special peak, the No. 6 peak is red sage root and licorice shared peaks, and the No. 7 peak is erigeron breviscapus and licorice shared peaks. The total length of the map is 65min.
The erigeron breviscapus medicinal material characteristic map established by adopting the method of the embodiment 1 has retention time t (14.9001), t (16.5201), t (21.5976), t (23.2657) and t (26.7667) of characteristic peaks in the erigeron breviscapus medicinal material characteristic map.
The characteristic spectrum of the red sage root medicine material established by the method in the embodiment 1 has retention times t (14.8718), t (21.5285), t (23.2254) and t (25.5043) of characteristic peaks in the characteristic spectrum of the red sage root medicine material.
The characteristic spectrum of the pseudo-ginseng medicinal material established by the method of the embodiment 1 is characterized in that the retention time t (21.7887), t (23.4867) and t (24.4002) of characteristic peaks in the characteristic spectrum of the pseudo-ginseng medicinal material.
The characteristic spectrum of the kudzuvine root medicinal material established by the method of the embodiment 1 is characterized by the times t (14.9651), t (21.5938) and t (23.2820) of characteristic peaks in the characteristic spectrum of the kudzuvine root medicinal material.
The characteristic spectrum of the licorice medicinal material established by the method of the embodiment 1 is characterized in that the retention time t (21.6025), t (23.2994), t (25.5568) and t (26.8003) of characteristic peaks in the characteristic spectrum of the licorice medicinal material.
Example 2 purple light tablet fingerprint establishment
Measurement of a total of 10 different batches of purple light chip test sample solutions by the method described in example 1 (lot numbers: 180601, 180701, 191101, 191102, 191201, 191202, 191203, 200101, 200202, 200301)
The similarity evaluation was performed on 10 batches of purple light sheets using "traditional Chinese medicine chromatography fingerprint similarity evaluation system" 2012 edition, and the similarity between 10 batches of purple light sheets and the control fingerprint (common mode S1 generated by 10 batches of purple light sheets) was greater than 0.99 (Table 1)
Table 1 ten batches of finger print similarity evaluation
Figure BDA0002649835210000042
Figure BDA0002649835210000051
Methodological verification
1. Precision test
The method of the embodiment 1 is adopted for measurement, the same part of the ultraviolet lamp chip sample solution is taken, six times of continuous sample injection (common mode S1 generated by six times of sample injection) are carried out, the obtained spectrum is imported into the traditional Chinese medicine chromatographic fingerprint similarity evaluation system software 2012 edition, and the similarity is calculated. The relative retention time of each chromatographic peak was calculated using the peak ginsenoside Rg1 No. 6 as a reference peak, and the results are shown in Table 2 and Table 3. The result shows that the similarity of the sample is above 0.99, and the relative retention time RSD of each characteristic peak is 0.01-0.06, which indicates that the method has good precision.
TABLE 2 evaluation of precision similarity
Figure BDA0002649835210000052
TABLE 3 precision vs. retention time
Figure BDA0002649835210000053
/>
Figure BDA0002649835210000061
2. Repeatability test
By the method of the embodiment 1, 6 parts of the purple light tablet sample solution is prepared in parallel for measurement (a common mode S1 generated by six parts of the samples), the obtained spectrum is imported into "2012 edition of Chinese medicine chromatography fingerprint similarity evaluation System software", and the similarity is calculated. The relative retention time of each chromatographic peak was calculated using the peak ginsenoside Rg1 No. 6 as a reference peak, and the results are shown in Table 4 and Table 5. The results show that the similarity of the test solutions of 6 parts of purple light tablets prepared in parallel is above 0.9, and the relative retention time RSD of each characteristic peak is 0.01-0.73, which indicates that the method has good repeatability.
Table 4 evaluation of repeatability similarity
Figure BDA0002649835210000062
TABLE 5 repeatability versus retention time
Figure BDA0002649835210000063
Figure BDA0002649835210000071
3. Solution stability test
The same portion of the test solution was taken and measured after 0, 2, 4, 8, 12, and 24 hours by the method described in example 1. The area of the chromatographic peak of ginsenoside Rg1 was calculated, and the relative retention time of each chromatographic peak was calculated by using the ginsenoside Rg1 of No. 6 peak as a reference peak, and the results are shown in Table 6 and Table 7. The results show that the same part of the ultraviolet lamp chip sample solution is measured after 0, 2, 4, 8, 12 and 24 hours, the RSD value of the ginsenoside Rg1 chromatographic peak is 0.63, the relative retention time RSD of each characteristic peak is 0.12-0.86, and the method has good stability within 24 hours.
TABLE 6 solution stability ginsenoside Rg1 peak area
Figure BDA0002649835210000072
TABLE 7 solution stability versus retention time
Figure BDA0002649835210000073
/>

Claims (3)

1. The HPLC fingerprint detection method of the purple light tablet is characterized by comprising the following steps:
step 1, preparing a sample solution:
precisely weighing 1g of the content of the purple lamp slice, placing the purple lamp slice into a conical bottle with a plug, precisely adding 25-50 ml of water-saturated n-butanol, weighing, carrying out reflux extraction for 2-3 hours, taking out, cooling, supplementing the reduced weight with the water-saturated n-butanol, filtering, precisely weighing 15-25 ml of a subsequent filtrate, placing the filtrate into a separating funnel, washing with ammonia test solution for 2 times, each time 25ml, discarding the ammonia test solution, evaporating the n-butanol solution to dryness, dissolving residues with methanol, concentrating to 10-15 ml, filtering with a microporous filter membrane, and obtaining a subsequent filtrate to obtain a test solution;
step 2, preparing a reference substance solution:
taking 5-15 mg of ginsenoside Rg1 and ginsenoside Rb1 reference substances respectively, placing into 50ml volumetric flasks, adding methanol to a certain volume to scale, shaking uniformly, filtering with microporous membrane, and collecting the subsequent filtrate to obtain reference substance solution;
step 3, chromatographic conditions:
ODS C 18 4.6mm X250 mm,5 μm column; mobile phase a is acetonitrile; mobile phase B is aqueous solution; the detection wavelength is 203nm; column temperature: 10-30 ℃; flow rate: 1.0ml . min -1 The elution procedure is a gradient elution procedure; wherein the gradient elution procedure is performed with the following volume to concentration configuration:
Figure FDA0003976708360000011
step 4, measuring:
and precisely sucking 10-20 mu l of the sample solution, injecting into a liquid chromatograph, and measuring by high performance liquid chromatography to obtain the fingerprint of the purple light tablet.
2. The method for detecting the HPLC fingerprint of the purple light chip according to claim 1, which is characterized in that:
step 1, preparing a sample solution:
precisely weighing 1g of the content of the purple lamp slice, placing the purple lamp slice into a conical bottle with a plug, precisely adding 50ml of water-saturated n-butanol, weighing, reflux-extracting for 2 hours, taking out, cooling, supplementing the reduced weight with the water-saturated n-butanol, filtering, precisely weighing 25ml of continuous filtrate, placing into a separating funnel, washing for 2 times with ammonia test solution, each 25ml of the ammonia test solution, discarding the ammonia test solution, evaporating the n-butanol solution, dissolving residues in methanol, concentrating to 10ml, filtering with a microporous filter membrane, and taking the continuous filtrate to obtain a sample solution;
step 2, preparing a reference substance solution:
taking 10mg of ginsenoside Rg1 reference substance and 7.5mg of ginsenoside Rb1 reference substance, respectively placing into 50ml volumetric flasks, adding methanol to constant volume to scale, shaking, filtering with microporous membrane, and collecting the subsequent filtrate to obtain reference substance solution;
step 3, chromatographic conditions:
ODS C 18 4.6mm X250 mm,5 μm column; mobile phase C is acetonitrile; mobile phase A is aqueous solution; the detection wavelength is 203nm; column temperature: 20 ℃; flow rate: 1.0ml . min -1 ；
Step 4, measuring:
and precisely sucking 10 mu l of the sample solution, injecting into a liquid chromatograph, and measuring by using a high performance liquid chromatography to obtain the fingerprint of the purple light slice.
3. The HPLC fingerprint detection method of the purple light patch according to claim 2, wherein: the fingerprint of the purple light tablet has 11 characteristic common peaks, wherein ginsenoside Rg1 is No. 6 peak, retention time is 25.5424 min, and ginsenoside Rb1 is No. 8 peak, and retention time is 33.9732 min.
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