CN110068640B - HPLC fingerprint spectrum-based quality detection method for Mongolian medicine pterocarpus santalinus heart medicinal material - Google Patents
HPLC fingerprint spectrum-based quality detection method for Mongolian medicine pterocarpus santalinus heart medicinal material Download PDFInfo
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Abstract
The invention discloses a quality detection method of a Mongolian medicine pterocarpus santalinus heart medicinal material based on an HPLC fingerprint, which comprises the following operation steps: step (1): preparing a test solution; step (2): injecting the sample solution prepared in the step (1) into a high performance liquid chromatograph for detection to obtain a sample chromatogram; and (3): preparing a control solution; and (4): injecting the control solution prepared in the step (3) into a high performance liquid chromatograph for detection to obtain a control fingerprint spectrum; and (5): and (3) comparing the chromatogram of the test sample obtained in the step (2) with the comparison fingerprint obtained in the step (4), and calculating the relative standard deviation RSD%. The method can be used as a means for identifying the authenticity and detecting the quality of the pterocarpus santalinus drug, and has the advantages of safety, reliability and controllable quality.
Description
The technical field is as follows:
the invention relates to a quality detection method of a pterocarpus santalinus heart medicinal material, in particular to a quality detection method of a Mongolian medicine pterocarpus santalinus heart medicinal material based on an HPLC fingerprint.
Background art:
the Pterocarpus santalinus used as Mongolian medicinal material is a clinical high-frequency medicine for Mongolian medicine, and is powder of dried heartwood of Pterocarpus indicus Willd, Pterocarpus indicus, which is a butterfly plant, is originally produced in various places from India to southeast Asia, and is also cultivated in Yunnan, Hainan and other places in China; alias: pterocarpus indicus, rosewood, dracaena cochinchinensis and the like. The heart wood is used as the medicine application part and has the efficacies of clearing blood heat, conditioning the hero's blood and diminishing swelling. It is mainly used for treating blood heat, blood stasis and stabbing pain, Hongyi (Hongyu) Hongchong (Chinese character of 'Baorii' heat), liver fire, heart heat and lump.
At present, the quality of the pterocarpus santalinus medicinal material is usually detected by an infrared spectroscopy, but because infrared spectrum data obtained by the method is a spectrogram, the similarity can not be calculated by data processing by software of a traditional Chinese medicine chromatography fingerprint similarity evaluation system (2004 edition, edited by the national pharmacopoeia committee), only source file data of infrared spectrograms of all pterocarpus santalinus samples can be copied from a workstation of a BRUKER IFS-55 type Fourier infrared spectrometer and then transferred to a TXT file, then the TXT file is imported into a word and transferred to an Excel, and the similarity is calculated by a specific calculation formula; therefore, a long calculation time is required, which lengthens the period of quality inspection and is not favorable for actual quality control.
The invention content is as follows:
the invention aims to provide a safe and effective quality detection method for a Mongolian medicine pterocarpus santalinus heart medicinal material based on an HPLC fingerprint.
The invention is implemented by the following technical scheme:
the quality detection method of the Mongolian medicine pterocarpus santalinus heart medicinal material based on the HPLC fingerprint comprises the following operation steps:
step (1): preparation of a test solution: grinding lignum Pterocarpi Indici into powder, extracting with 70% ethanol solution, filtering the extractive solution, and preparing into test solution;
step (2): injecting the test solution prepared in the step (1) into a high performance liquid chromatograph for detection to obtain a test chromatogram;
and (3): preparation of control solution: grinding lignum Pterocarpi Indici reference medicinal material into powder, extracting with 70% ethanol solution, filtering the extractive solution, and preparing reference solution;
and (4): injecting the control solution prepared in the step (3) into a high performance liquid chromatograph for detection to obtain a control fingerprint spectrum;
and (5): and (3) comparing the chromatogram of the test sample obtained in the step (2) with the reference fingerprint obtained in the step (4), and calculating the relative standard deviation RSD%, wherein the medicinal material with the relative standard deviation RSD% less than or equal to 5% is the positive Mongolian medicine pterocarpus santalinus heart medicinal material.
Further, the chromatographic conditions of the step (2) and the step (4) are as follows:
a chromatographic column: octadecyl bonding silica gel column; detection wavelength: 380 plus or minus 3 nm; the flow rate is 0.8-1.2 mL/min; the column temperature is 40 +/-5 ℃; the sample amount is 10 mul;
using acetonitrile-0.02% phosphoric acid water solution as mobile phase to carry out gradient elution, wherein the gradient elution procedure is as follows: the concentration of the mobile phase is changed into 0min, 10% acetonitrile; 0-10 min, 10% -25% acetonitrile; 10-30 min, 25% acetonitrile; 30-50 min, 25% -30% acetonitrile; 50-70 min, 30-70% acetonitrile; 70-71 min, 70% -10% acetonitrile.
Further, the size of the column is 250mm × 4.6mm, 5 μm.
Further, the chromatographic column is a Thermo C18 column.
Further, the detection wavelength was 380 nm.
Further, the flow rate was 1.0 ml/min.
Further, the column temperature was 40 ℃.
Further, in the step (1) and the step (3), the extraction method is ultrasonic.
Furthermore, the contrast fingerprint spectrum has 17 common peaks, the positive Mongolian medicine pterocarpus santalinus heart medicinal material is used as contrast, and the retention time of each common peak is as follows: peak 1: 4.2306min, Peak 2: 5.8878 min; peak 3: 7.3054 min; peak 4: 8.5168 min; peak 5: 9.1734 min; peak 6: 10.8960 min; peak 7: 11.1184 min; peak 8: 13.5080 min; peak 9: 14.3328 min; peak 10: 21.3498 min; peak 11: 28.2706 min; peak 12: 32.1500 min; peak 13: 36.5248 min; peak 14: 50.6506 min; peak 15: 52.7486 min; peak 16: 56.8832 min; peak 17: 60.5084 min.
Further, the peak area of each common peak in the control fingerprint is as follows: peak 1: 0.0767 to 0.0728; peak 2: 0.4079-0.3866; peak 3: 0.3591-0.3596; peak 4: 1.5613 to 1.5642; peak 5: 0.2649-0.2685; peak 6: 0.1880-0.1859; peak 7: 0.5311-0.5338; peak 8: 0.4035-0.4118; peak 9: 0.2041-0.2007; peak 10: 4.0967-4.0257; peak 11: 14.3176-14.3658; peak 12: 6.9717-6.9678; peak 13: 10.0338-10.0040; peak 14: 5.9021-5.9283; peak 15: 59.2227-59.2090; peak 16: 17.2560-17.2297; peak 17: 1.5852-1.5200.
The invention has the advantages that:
according to the invention, 10 batches of lignum pterocarpi indici medicinal material samples are detected, the obtained fingerprint spectrums have similarity but are not completely consistent, the overall appearances of main peak groups are basically consistent, and the peak areas of all the components are different. The reason is considered to be related to factors such as the ecological environment of the producing area. The quality of the medicinal materials can be comprehensively and comprehensively judged by combining the fingerprint spectrum with the principal component analysis.
According to the method provided by the invention, the accuracy of analysis is improved by comprehensively evaluating 17 substances represented by 17 common peaks; the detection amount of the liquid phase required by the method is small, so that the method has high detection sensitivity and does not need to prepare a large amount of detection solution; data processing is carried out by adopting software of 'Chinese medicine chromatogram fingerprint similarity evaluation system 2004 version A' (compiled by the State pharmacopoeia Committee), and a spectrogram capable of comprehensively reflecting common characteristics of a plurality of chromatograms can be obtained by comparing the plurality of chromatograms; the calculation speed is high, the detection period is short, and the high-efficiency advantage is achieved; the High Performance Liquid Chromatography (HPLC) fingerprint spectrum can be used for qualitatively identifying the authenticity of the pterocarpus santalinus and quantitatively analyzing the quality of the pterocarpus santalinus, can be used as an effective means for identifying the authenticity and detecting the quality of the pterocarpus santalinus, and has the advantages of safety, reliability and controllable quality.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a finger print of lignum Pterocarpi Indici control medicinal material;
FIG. 2 is a finger print of lignum Pterocarpi Indici;
FIG. 3 is an overlay of precision test fingerprints of lignum Pterocarpi Indici;
FIG. 4 is an overlay of the stability test fingerprints of lignum Pterocarpi Indici;
FIG. 5 is an overlay of the repeatability test fingerprints of lignum Pterocarpi Indici;
fig. 6 is a fingerprint of 10 batches of lignum pterocarpi indici medicinal materials.
The specific implementation mode is as follows:
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.
Example 1:
instruments and materials:
thermo 3000 high performance liquid chromatograph, the semer flies the autosampler, diode array detector, ultrasonic cleaner: model, KQ3200DV model number, kunshan ultrasonic instruments ltd; universal high-speed disintegrator, model: FLB-500A, Shanghai Philibo food machinery, Inc.; ultrapure water making machine, model: XJG-40-B, Shenyang Xinjie science and technology Co., Ltd; electric hot blast drying ovens (shanghai-heng science instruments ltd); AL104 electronic balance (mettler-toledo instruments ltd), column Thermo C18(250 × 4.6mm5 μm); lignum Pterocarpi Indici (batch number: 20100829, 20100830, 20120920, 1203011), provided by Mongolian medicine preparation center of China; (batch Nos.: 20100203, 100501, 20140513), purchased from different local drugstores; indian red sandalwood core (batch number: 20150618, 20150714) purchased from beads market in Hoohait; the reference substance is a certified Mongolian medicine pterocarpus santalinus heart medicinal material (the batch numbers are 121310-200301 respectively) purchased from a China pharmaceutical and biological product certification institute; analytically pure formic acid (jin dong tian zheng fine chemical reagent factory, Tianjin); phosphoric acid, analytically pure (jin Dongtianzheng fine chemical reagent factory, Tianjin); absolute ethanol, analytically pure (jin dong tian zheng fine chemical reagent factory, Tianjin city); acetonitrile, chromatographically pure (beijing yinoka science ltd); ultrapure water and distilled water, and is prepared by self.
The quality detection method of the Mongolian medicine pterocarpus santalinus heart medicinal material based on the HPLC fingerprint spectrum in the embodiment 1 comprises the following operation steps:
(1) establishing an HPLC fingerprint spectrum of the santalum album reference medicinal material: taking 0.5g of lignum Pterocarpi Indici as a reference medicinal material, precisely weighing, placing into a conical flask with a plug, adding 10ml of 70% ethanol solution, precisely weighing, ultrasonically treating for 30min, taking out, cooling, precisely weighing again, filling the weight loss with 70% ethanol after 2 times of weight loss difference, standing, and filtering. Filtering the filtrate with microporous membrane to obtain lignum Pterocarpi Indici control solution. Selecting the detection at 380nm wavelength; injecting 10 μ l sample, and referring to the fingerprint of the medicinal material shown in figure 1.
(2) Preparation of a test solution: pulverizing lignum Pterocarpi Indici into coarse powder, sieving with No. 3 sieve, collecting powder 0.5g, precisely weighing, placing into conical flask with plug, adding 70% ethanol 10ml, sealing, precisely weighing, ultrasonic treating for 30min, taking out, cooling, precisely weighing again, filling the weight loss with 70% ethanol for 2 times, standing, and filtering. Filtering the filtrate with microporous membrane to obtain test solution.
(3) Injecting the test solution into a high performance liquid chromatograph, and detecting under the following chromatographic conditions: a chromatographic column: thermo C18 column (250 mm. times.4.6 mm, 5 μm); detection wavelength: 380 nm; the flow rate is 1.0 mL/min; the column temperature is 40 ℃; the sample amount is 10 mul;
using acetonitrile-0.02% phosphoric acid water solution as mobile phase to carry out gradient elution, wherein the gradient elution procedure is as follows: the concentration of the mobile phase is changed into 0min, 10% acetonitrile; 0-10 min, 10% -25% acetonitrile; 10-30 min, 25% acetonitrile; 30-50 min, 25% -30% acetonitrile; 50-70 min, 30-70% acetonitrile; 70-71 min, 70% -10% acetonitrile. The finger print of the test sample is shown in figure 2.
After detection, the obtained test sample fingerprint is compared with the reference drug fingerprint, and the drug with the relative standard deviation RSD percent less than or equal to 5 percent is the certified Mongolian drug pterocarpus santalinus heart drug.
Example 2:
1. the sources of the lignum pterocarpi indici medicinal material samples used in the material experiments are shown in table 1.
TABLE 1 Mongolian medicinal material lignum pterocarpi indici HPLC fingerprint sample batch Table
| Zisantal medicinal material number | Sample numbering | Batch number | Source |
| 1 | S1 | 9814104 | Mongolian medicine room supply of inner Mongolian food and |
| 2 | S2 | 20100203 | Purchased from a Furui big pharmacy store, Hui city: is not detailed in |
| 3 | S3 | 100501 | Purchased in the large pharmacy of the He Xianchang, Hui city: hainan province |
| 4 | S4 | 20100829 | Purchased from shou chun hall pharmacies in respiratory city: is not detailed in |
| 5 | S5 | 20100830 | The national center for Mongolian preparations provides the production area: guangdong (Chinese character of Guangdong) |
| 6 | S6 | 1203011 | The national center for Mongolian preparations provides the production area: guangdong (Chinese character of Guangdong) |
| 7 | S7 | 20140513 | Purchased from shou chun hall pharmacies in respiratory city: guangdong (Chinese character of Guangdong) |
| 8 | S8 | 20150806 | The pterocarpus indicus heartwood is purchased from the production places of the Buddha bead market in Hui city: guangdong (Chinese character of Guangdong) |
| 9 | S9 | 20150916 | Purchased from shou chun hall pharmacies in respiratory city: guangdong (Chinese character of Guangdong) |
| 10 | S10 | 121310-200301 | Lignum Pterocarpi Indici reference medicinal material purchased from China institute for testing biological products |
2. Method and results
2.1 chromatographic conditions
A chromatographic column: thermo C18 column (250 mm. times.4.6 mm, 5 μm); detection wavelength: 380 nm; the flow rate is 1.0 mL/min; the column temperature is 40 ℃; the sample amount is 10 mul; using acetonitrile-0.02% phosphoric acid water solution as mobile phase to carry out gradient elution, wherein the gradient elution procedure is as follows: the concentration of the mobile phase is changed into 0min, 10% acetonitrile; 0-10 min, 10% -25% acetonitrile; 10-30 min, 25% acetonitrile; 30-50 min, 25% -30% acetonitrile; 50-70 min, 30-70% acetonitrile; 70-71 min, 70% -10% acetonitrile.
2.2, preparation of a reference solution:
taking 0.5g of lignum Pterocarpi Indici as a reference medicinal material, precisely weighing, placing into a conical flask with a plug, adding 10ml of 70% ethanol solution, precisely weighing, ultrasonically treating for 30min, taking out, cooling, precisely weighing again, filling the weight loss with 70% ethanol after 2 times of weight loss difference, standing, and filtering. Filtering the filtrate with microporous membrane to obtain lignum Pterocarpi Indici control solution.
2.3, preparation of a test solution: pulverizing lignum Pterocarpi Indici into coarse powder, sieving with No. 3 sieve, collecting powder 0.5g, precisely weighing, placing into conical flask with plug, adding 70% ethanol 10ml, sealing, precisely weighing, ultrasonic treating for 30min, taking out, cooling, precisely weighing again, filling the weight loss with 70% ethanol for 2 times, standing, and filtering. Filtering the filtrate with microporous membrane to obtain test solution.
2.4 methodology examination
2.4.1, precision test
And continuously sampling the same sample solution for 6 times, and recording chromatograms, wherein the RSD of the retention time of 17 chromatographic peaks is less than or equal to 5%, and the retention time of the obtained chromatographic peaks is within +/-1 min of the average retention time. The results are shown in FIG. 3 and Table 2, which show that the HPLC apparatus used in this example is accurate.
TABLE 2 Mongolian medicine Pterocarpus santalinus precision test peak area RSD%
2.4.2 stability test
Taking the same sample solution, respectively injecting samples at 0,2,4,8 and 12 hours for measurement, taking the peak area and retention time of the characteristic fingerprint as standards, and investigating the stability of the sample, wherein the results are shown in a figure 4 and a table 3, and the RSD of the retention time of all the shared peaks is less than or equal to 5%, which indicates that the stability of the sample in 12 hours is good.
TABLE 3 Mongolian medicine Pterocarpus santalinus stability test Peaarea RSD%
2.4.3 repeatability tests
Accurately weighing 5 parts of the lignum pterocarpi indici medicinal material of the same batch, each 0.5g, placing in a conical flask with a bottle stopper, adding 10ml of 70% ethanol, weighing, performing ultrasonic treatment for 30min, taking out, cooling, accurately weighing again, filling the weight loss difference for 2 times with 70% ethanol, standing, and filtering. Filtering the filtrate with microporous membrane to obtain test solution. And (3) sampling each sample for 1 time to obtain a plurality of chromatographic peaks of the characteristic fingerprint, wherein the peak area RSD% of the chromatographic peaks is less than or equal to 5%, and the retention time of the obtained chromatographic peaks is within +/-1 min of the average retention time. The results are shown in Table 4 of FIG. 5, which shows that the method adopted in this example has good reproducibility and meets the requirements of fingerprint.
TABLE 4 Mongolian medicine Pterocarpus santalinus repeatability test peak area RSD%
2.5 sample determination
The sample solutions were prepared under item "2.3" for each batch, analyzed under the chromatographic conditions under item "2.1", and the chromatograms at 75min were recorded.
2.6 establishment of characteristic fingerprint and technical parameters
Precisely sucking 10 μ l of test solutions of lignum Pterocarpi Indici from different sources, and analyzing by sample injection, wherein the serial numbers of the lignum Pterocarpi Indici and the samples are shown in Table 4. According to HPLC detection of 10 batches of test samples of lignum pterocarpi indici medicinal materials with different sources, the fingerprint of the test sample is compared with the fingerprint of a control, and the result shows that when the wavelength is 380nm, 17 peaks are the common peaks of all the batches of medicinal materials, the peak area is stable, and the peak shape is good, so the peaks are used as the 17 common peaks, and the fingerprint of the 17 common peaks is established, as shown in figure 6.
The data processing method comprises the following steps: the similarity of the fingerprints of all batches of the santalum album linn medicinal materials and the comparison fingerprints is evaluated by software of a Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition (compiled by the State pharmacopoeia Committee), the result is shown in Table 5, the similarity is between 0.85 and 0.999, and the result shows that the chemical components are basically the same, but the quantity of the chemical components is different.
TABLE 5 similarity between finger print of lignum Pterocarpi Indici and the reference finger print of each batch
3. Conclusion
The experimental result shows that the fingerprint spectrums of 10 batches of the pterocarpus santalinus medicinal material samples have similarity but are not completely consistent, the overall appearances of main peak groups are basically consistent, but the peak areas of all the components are different. The reason is considered to be related to factors such as the producing area and the ecological environment. The quality of the medicinal materials can be comprehensively and comprehensively judged by combining the fingerprint spectrum and the principal component analysis, so that the method can be used as a means for identifying the authenticity and detecting the quality of the pterocarpus santalinus.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The quality detection method of the Mongolian medicine pterocarpus santalinus heart medicinal material based on the HPLC fingerprint is characterized by comprising the following operation steps:
step (1): preparation of a test solution: grinding lignum Pterocarpi Indici into powder, extracting with 70% ethanol solution, filtering the extractive solution, and preparing into test solution;
step (2): injecting the test solution prepared in the step (1) into a high performance liquid chromatograph for detection to obtain a test chromatogram;
and (3): preparation of control solution: grinding lignum Pterocarpi Indici reference medicinal material into powder, extracting with 70% ethanol solution, filtering the extractive solution, and preparing reference solution;
and (4): injecting the control solution prepared in the step (3) into a high performance liquid chromatograph for detection to obtain a control fingerprint spectrum;
and (5): comparing the chromatogram of the test sample obtained in the step (2) with the reference fingerprint obtained in the step (4), and calculating the relative standard deviation RSD%, wherein the medicinal material with the relative standard deviation RSD% less than or equal to 5% is the positive Mongolian medicine pterocarpus santalinus heart medicinal material;
the chromatographic conditions of the step (2) and the step (4) are as follows:
a chromatographic column: octadecyl bonding silica gel column; detection wavelength: 380 plus or minus 3 nm; the flow rate is 0.8-1.2 mL/min; the column temperature is 40 +/-5 ℃; the sample amount is 10 mul;
using acetonitrile-0.02% phosphoric acid water solution as mobile phase to carry out gradient elution, wherein the gradient elution procedure is as follows: the concentration of the mobile phase is changed into 0min, 10% acetonitrile; 0-10 min, 10% -25% acetonitrile; 10-30 min, 25% acetonitrile; 30-50 min, 25% -30% acetonitrile; 50-70 min, 30-70% acetonitrile; 70-71 min, 70% -10% acetonitrile;
the size of the chromatographic column is 250mm multiplied by 4.6mm and 5 mu m;
the chromatographic column is a Thermo C18 column;
the detection wavelength is 380 nm;
the flow rate is 1.0 ml/min;
the column temperature was 40 ℃.
2. The quality detection method for the Mongolian medicine pterocarpus santalinus drug based on the HPLC fingerprint spectrum as claimed in claim 1, wherein in the step (1) and the step (3), the extraction method is ultrasonic.
3. The quality detection method for the Mongolian medicine pterocarpus santalinus drug based on the HPLC fingerprint spectrum as claimed in claim 1, wherein the contrast fingerprint spectrum has 17 common peaks, the quality Mongolian medicine pterocarpus santalinus drug is used as a contrast, and the retention time of each common peak is as follows: peak 1: 4.2306min, Peak 2: 5.8878 min; peak 3: 7.3054 min; peak 4: 8.5168 min; peak 5: 9.1734 min; peak 6: 10.8960 min; peak 7: 11.1184 min; peak 8: 13.5080 min; peak 9: 14.3328 min; peak 10: 21.3498 min; peak 11: 28.2706 min; peak 12: 32.1500 min; peak 13: 36.5248 min; peak 14: 50.6506 min; peak 15: 52.7486 min; peak 16: 56.8832 min; peak 17: 60.5084 min.
4. The quality detection method for the Mongolian medicine pterocarpus santalinus drug based on the HPLC fingerprint spectrum as claimed in claim 3, wherein the peak area of each common peak in the control fingerprint spectrum is: peak 1: 0.0767 to 0.0728; peak 2: 0.4079-0.3866; peak 3: 0.3591-0.3596; peak 4: 1.5613 to 1.5642; peak 5: 0.2649-0.2685; peak 6: 0.1880-0.1859; peak 7: 0.5311-0.5338; peak 8: 0.4035-0.4118; peak 9: 0.2041-0.2007; peak 10: 4.0967-4.0257; peak 11: 14.3176-14.3658; peak 12: 6.9717-6.9678; peak 13: 10.0338-10.0040; peak 14: 5.9021-5.9283; peak 15: 59.2227-59.2090; peak 16: 17.2560-17.2297; peak 17: 1.5852-1.5200.
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