CN110988206A - Quality evaluation method of morinda officinalis - Google Patents
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Abstract
The invention provides a quality evaluation method of morinda officinalis. The quality evaluation method of morinda officinalis comprises the following steps: preparing a mixed reference substance solution; positioning a chromatographic peak of a component to be detected; calculating a relative correction factor; and (4) measuring the content of the sample, and establishing a multi-evaluation quality evaluation method for morinda officinalis. According to the method, accurate positioning of the chromatographic peak of each component to be measured is realized through calculation of relative retention time, and by means of specific chromatographic conditions, simultaneous measurement of a plurality of components can be realized only by measuring the content of one component of the deacetylated asperulosidic acid, so that the aim of controlling the overall quality of the traditional Chinese medicine is fulfilled, a one-measurement-multiple-evaluation quality control system of the morinda officinalis traditional Chinese medicinal materials is reduced, data processing is simplified, and the method is simple to operate, economical and efficient. The RSD values of the relative correction factors of the chromatographic systems and chromatographic columns of different models are less than 2%, the RSD values of the relative retention times of the chromatographic systems and chromatographic columns of different models are less than 4%, the reproducibility is good, and the detection reproducibility and the stability are good.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine analysis, and more particularly relates to a quality evaluation method of morinda officinalis.
Background
The quality of the traditional Chinese medicine directly influences the effect of dialectical treatment in the clinical traditional Chinese medicine, so that the effective control of the quality of the traditional Chinese medicine is the premise of ensuring the clinical curative effect of the traditional Chinese medicine. The complex diversity of the traditional Chinese medicine components determines that the single component can not accurately realize the quality control of the traditional Chinese medicine, the research mode of the single active component of the chemical medicine is directly applied to the traditional Chinese medicine, the traditional Chinese medicine composition completely deviates from the treatment concept of 'prescription-syndrome-effect' of the traditional Chinese medicine, and the overall regulation effect of multiple targets and multiple ways of the traditional Chinese medicine is ignored, so that the quality of the multiple components of the traditional Chinese medicine is required to be controlled and detected, and the quality control of multiple indexes is realized. The traditional multi-index synchronous quality control needs various traditional Chinese medicine multi-reference products, and due to the large separation difficulty of the reference products, the shortage of the goods sources and the high detection cost, the multi-index quality evaluation mode is mostly used for scientific research and less used for actual quality monitoring.
The content measurement item of morinda officinalis in 2015 version of Chinese pharmacopoeia adopts acesulfame as a quantitative index, so that certain limitation exists, and if various index components can be brought into the quantitative index, the quality of morinda officinalis can be comprehensively evaluated. Traditional multi-index synchronous quality control of morinda officinalis medicinal materials requires multiple traditional Chinese medicine reference substances, and due to the fact that the reference substances are high in separation difficulty, short in supply of goods and high in detection cost, a multi-index quality evaluation mode is rarely used for actual quality supervision. CN103884676A discloses a method for rapidly determining the content of multi-index components in traditional Chinese medicinal materials, which is characterized in that the content of the multi-index components in the traditional Chinese medicinal materials is rapidly determined by near infrared spectroscopy, but the disclosed multi-index determination method is actually to respectively determine the content of water and soluble solids by a drying method, determine the content of hypoxanthine by a high performance liquid chromatography, determine the content of free amino acid and polypeptide by a high performance liquid chromatography pre-column derivatization method, determine the content of total sugar and polysaccharide by an iodine solution-sodium thiosulfate titration method, achieve the purpose of multi-index detection by establishing a quantitative analysis model for each determination data, still is similar to the traditional detection method, and can not realize the quantitative detection of multiple quality indexes by one-time detection, thereby establishing a multi-index quality evaluation mode. In addition, the existing traditional Chinese medicine quality evaluation methods do not disclose a multi-index quality evaluation method of related specific morinda officinalis, in particular the quality control of morinda officinalis by one-test multi-evaluation method.
Disclosure of Invention
The invention aims to solve the technical problems that the multi-index synchronous quality control of traditional morinda officinalis traditional Chinese medicinal materials needs multiple traditional Chinese medicines and multiple photographs, and is not economical, simple and efficient, and provides a quality evaluation method of morinda officinalis.
The above purpose of the invention is realized by the following technical scheme:
a quality evaluation method of radix Morindae officinalis comprises the following steps:
s1, preparing a mixed reference solution: preparing a mixed reference solution of the monotropein, the deacetyl asperulosidic acid, the asperulosidic acid and the asperuloside;
s2, positioning of a chromatographic peak of a component to be detected: calculating the relative retention time of each component to be detected in the mixed reference substance relative to the deacetyl asperulosidic acid by taking the deacetyl asperulosidic acid as an internal reference substance, and determining the positioning of the chromatographic peak of the component to be detected by adopting the relative retention time;
s3, calculating a relative correction factor: determining high performance liquid chromatography peaks of the components in the mixed reference substance according to the positioning of the chromatography peaks, taking deacetylated asperuloside as an internal reference substance, and respectively calculating relative correction factors of the monotropein, the asperuloside and the asperuloside according to peak areas of the chromatography peaks of the components in the mixed reference substance;
s4, sample content determination: using deacetyl asperuloside as an internal reference, determining the peak area of a chromatographic peak of a sample to be tested by using a high performance liquid phase, calculating the mass contents of the monotropein, the asperuloside and the asperuloside in morinda officinalis according to relative correction factors, establishing a multi-evaluation quality evaluation method for morinda officinalis,
wherein the conditions of the liquid chromatography are as follows: mobile phase: acetonitrile A, acetonitrile B: 0.01moL of dipotassium hydrogen phosphate + 0.2% phosphoric acid solution, the chromatographic conditions can influence the resolution of chromatographic peaks, thereby influencing the peak area of chromatographic peaks and finally influencing the content determination result.
Gradient elution: 0-12min, 1% A; 12-30min, 1% -A-17% A; 30-40min, 17% A;
flow rate: 1.0 mL/min-1；
Detection wavelength: 235 nm;
column temperature: 25 ℃; sample introduction amount: 20 μ L.
A QAMS (quantitative analysis of multi-compounds by single-marker) realizes synchronous measurement of a plurality of components (the reference substances are difficult to obtain or supply) by measuring one component (the reference substances are easy to obtain) by utilizing the internal function and the proportional relation among the effective components of the traditional Chinese medicines, is a multi-index quality evaluation mode suitable for the characteristics of the traditional Chinese medicines, and has not been applied to the quality control of the medicinal indianmulberry root.
Compared with the traditional multi-index synchronous quality control method, the one-test multi-evaluation method simplifies data processing, reduces cost, and has the characteristics of economy, high efficiency and simplicity. The key factors influencing the repeatability and the accuracy of the one-test multi-evaluation method are the positioning of a chromatographic peak of a component to be tested and the determination of a relative correction factor. The selection of the peak positioning mode of the component to be detected directly influences the accuracy of the response value of the detector and is also a key factor influencing the accuracy of the one-detection multi-evaluation method.
Wherein, the calculation formula of the relative correction factor is as follows: f. ofk/s＝(Cs×Ak)/(Ck×As)
fk/sIs a relative correction factor;
Csthe mass concentration of the internal reference;
Asthe peak area of the internal reference substance is shown;
Ckthe mass concentration of the component to be measured;
Akthe peak area of the component to be measured;
deacetyl asperuloside is used as an internal reference.
Wherein, the calculation formula of the relative retention time is as follows: rtR＝tRk/tRs
RtRIs the relative retention time;
tRkthe retention time of the internal reference substance deacetyl asperuloside is shown;
tRsis the retention time of the component to be measured.
Preferably, the chromatographic column of the liquid chromatography is a Venusil MP C18 chromatographic column or an Agilent ZORBAX SB-Aq chromatographic column, and the size of the chromatographic column is as follows: 250 mm. times.4.6 mm, 5 μm.
Preferably, the relative correction factor in S3 is the average value of the relative correction factors for the mixed control solution sample volumes of 5. mu.L, 10. mu.L, 15. mu.L, 20. mu.L and 30. mu.L.
Preferably, the relative correction factor of the monotropein in S3 is 1.3948-1.4293, the relative correction factor of the asperuloside is 1.2638-1.2897, and the relative correction factor of the asperuloside is 1.3152-1.3245.
Preferably, the relative correction factor for monotropein in S3 is 1.4184, the relative correction factor for asperuloside is 1.2725, and the relative correction factor for asperuloside is 1.3211.
Preferably, the relative retention time of the monotropein in S2 is 0.7144-0.7483, the relative retention time of the asperuloside is 2.1531-2.3162, and the relative retention time of the asperuloside is 2.2926-2.4799.
Preferably, the relative retention time of monotropein in S2 is 0.7296, the relative retention time of asperuloside is 2.2179, and the relative retention time of asperuloside is 2.3858.
Preferably, the preparation method of the mixed control solution in S1 is specifically as follows: add the mixed control to the initial mobile phase: acetonitrile A, acetonitrile B: dissolving 0.01moL of dipotassium hydrogen phosphate and 0.2% phosphoric acid solution and fixing the volume, wherein the mass concentration of the monotropein is 0.6352 mg/mL-1，The mass concentration of the deacetyl asperuloside is 0.2100 mg/mL-1The mass concentration of the asperulosidic acid is 1.256 multiplied by 10-2mg·mL-1The mass concentration of asperuloside is 5.07 x 10-3mg·mL-1. The reference substances of the invention are: the four components are common iridoid components in medicinal indianmulberry root.
Preferably, the sample in S4 is prepared by the following method: weighing morinda officinalis sample powder, adding 80% methanol solution for ultrasonic extraction, filtering to obtain filtrate, evaporating the filtrate to dryness to obtain extract residue, and mixing the extract residue with an initial mobile phase: acetonitrile A, acetonitrile B: dissolving 0.01moL of dipotassium hydrogen phosphate and 0.2% of phosphoric acid solution, metering volume to obtain an extract residue solution, and filtering to obtain a test solution.
Preferably, the ultrasonic extraction time is 30min, the power is 400W, and the frequency is 90 HZ.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a quality evaluation method of morinda officinalis, which realizes accurate positioning of chromatographic peaks of components to be measured by calculating relative retention time, can realize simultaneous measurement of a plurality of components of monotropein, asperulosidic acid and asperuloside by only measuring the content of one component of deacetylated asperulosidic acid in cooperation with specific chromatographic conditions, finally achieves the purpose of controlling the overall quality of traditional Chinese medicines, reduces a one-measurement multi-evaluation quality control system of morinda officinalis traditional Chinese medicinal materials, simplifies data processing, and is simple in operation, economic and efficient.
The RSD values of the chromatographic systems and chromatographic columns of different models relative to the correction factor are less than 2%, and the reproducibility is good; the relative retention time RSD values of chromatographic systems and chromatographic columns of different models are less than 4%, the reproducibility is good, and the detection reproducibility and stability are good.
Drawings
FIG. 1 is a 3D absorption spectrum of monotropein.
FIG. 2 is a 3D absorption spectrum of deacetyl asperuloside.
FIG. 3 is a 3D absorption spectrum of asperuloside.
FIG. 4 is a 3D absorption spectrum of asperuloside.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A quality evaluation method of radix Morindae officinalis comprises the following steps:
s1, preparing a mixed reference solution: preparing a mixed reference solution of the monotropein, the deacetyl asperulosidic acid, the asperulosidic acid and the asperuloside;
s2, positioning of a chromatographic peak of a component to be detected: calculating the relative retention time of each component to be detected in the mixed reference substance relative to the deacetyl asperulosidic acid by taking the deacetyl asperulosidic acid as an internal reference substance, and determining the positioning of the chromatographic peak of the component to be detected by adopting the relative retention time;
s3, calculating a relative correction factor: determining high performance liquid chromatography peaks of the components in the mixed reference substance according to the positioning of the chromatography peaks, taking deacetylated asperuloside as an internal reference substance, and respectively calculating relative correction factors of the monotropein, the asperuloside and the asperuloside according to peak areas of the chromatography peaks of the components in the mixed reference substance;
s4, sample content determination: the method comprises the steps of taking deacetylated asperuloside as an internal reference, measuring the peak area of a chromatographic peak of a sample to be measured by utilizing a high performance liquid phase, calculating the mass contents of monotropein, asperuloside and asperuloside in morinda officinalis according to relative correction factors, and establishing a multi-evaluation morinda officinalis quality evaluation method.
Wherein the chromatographic instrument and chromatographic conditions are as follows:
agilent 1260 high performance liquid chromatograph; a chromatographic column: venusil MP C18 column (250 mm. times.4.6 mm, 5 μm); mobile phase: acetonitrile (A) -0.01moL of dipotassium hydrogen phosphate and 0.2 percent of phosphoric acid solution (B), and gradient elution (0-12min, 1 percent of A, 12-30min, 1 percent of A-17 percent of A, 30-40min, 17 percent of A); flow rate: 1.0mL min-1; detection wavelength: 235 nm; column temperature: 25 ℃; sample introduction amount: 20 μ L.
Preparation of control solutions:
accurately weighing appropriate amount of monoterpene with chloranthus glaucoside, deacetyl asperulosidic acid, asperulosidic acid and asperuloside, adding initial mobile phase (1% acetonitrile + 99% 0.01moL dipotassium hydrogen phosphate + 0.2% phosphoric acid solution) for dissolving and fixing volume to obtain final product with quality concentration of 0.6352 mg/mL-10.2100 mg/mL deacetyl asperuloside-1Asperuloside 1.256X 10-2mg·mL-1Asperuloside 5.07 x 10-3mg·mL-1The mixed reference solution is stored at low temperature in dark.
Preparation of test solution
Weighing about 0.5g of Morinda officinalis sample powder (sieved with 60 mesh sieve), placing into a conical flask with a plug, adding 100mL of 80% methanol solution, ultrasonically extracting for 30min (power is 400W, frequency is 90HZ), filtering, extracting the residue once again by the same method, and filtering. Mixing filtrates, and evaporating to obtain extract residue. The above extract residue was dissolved with an initial mobile phase (1% acetonitrile + 99% 0.01moL dipotassium hydrogen phosphate + 0.2% phosphoric acid solution) and the volume was determined to 10mL volumetric flask, and mixed well. Filtering with 0.45 μm microporous membrane, and collecting the filtrate to obtain the sample solution.
S2, positioning of a chromatographic peak of a component to be detected:
the method takes the deacetyl asperuloside as an internal reference substance, and takes the relative value of the retention time of the deacetyl asperuloside as the positioning standard of the component to be detected.
The formula for the relative retention time is: rtR＝tRk/tRs
RtRIs the relative retention time;
tRkthe retention time of the internal reference substance deacetyl asperuloside is shown;
tRsis the retention time of the component to be measured.
The specific relative retention times are: t is tⅠ/Ⅰ0.7277；tⅢ/Ⅰ2.237；tⅣ/Ⅰ2.4338。
Wherein, I is the monotropein; i is deacetyl asperuloside; III is asperulosidic acid; IV is asperuloside.
S3, calculating a relative correction factor:
calculating relative correction factor by using a multipoint correction method, precisely sucking 5 μ L, 10 μ L, 15 μ L, 20 μ L and 30 μ L of mixed reference substance solution, respectively injecting into a high performance liquid chromatograph, performing sample injection measurement according to chromatographic conditions, and respectively recording peak areas of chromatographic peaks of the components. Uses deacetyl asperuloside (I) as an internal reference substance,
the relative correction factor is calculated as: f. ofk/s＝(Cs×Ak)/(Ck×As)
fk/sIs a relative correction factor;
Csthe mass concentration of the internal reference;
Asthe peak area of the internal reference substance is shown;
Ckthe mass concentration of the component to be measured;
Akthe peak area of the component to be measured.
Relative correction factors of the monotropein (I), the asperuloside (III) and the asperuloside (IV) are respectively calculated, and the calculation results are shown in a table.
TABLE 1 relative correction factor
| Sample volume (μ L) | fⅠ/Ⅰ | fⅢ/Ⅰ | fⅣ/Ⅰ |
| 5 | 1.4293 | 1.2760 | 1.3245 |
| 10 | 1.4256 | 1.2897 | 1.3233 |
| 15 | 1.4236 | 1.2692 | 1.3244 |
| 20 | 1.4187 | 1.2638 | 1.3181 |
| 30 | 1.3948 | 1.2638 | 1.3152 |
| Mean value of | 1.4184 | 1.2725 | 1.3211 |
| RSD(％) | 0.97 | 0.85 | 0.32 |
Example 2 reproducibility examination with respect to correction factor
The influence of two different types of chromatographic systems Agilent 1260 and Waters E2695 and two different chromatographic columns Venusil MP C18 and Agilent ZORBAX SB-Aq (both 250mm multiplied by 4.6mm, 5 μm) on the relative correction factor is considered, and the relative correction factor and the RSD value thereof are respectively calculated, and the result is shown in Table 2.
TABLE 2 results of relative correction factor investigation of different instruments and columns
The relative correction factor RSD values using different instruments and columns were all less than 2%, indicating good reproducibility.
Example 3 reproducibility of relative Retention time
The effect of different instruments and columns on the relative retention times was examined and their RSD values were calculated and the results are shown in table 3.
TABLE 3 examination of the relative retention times of the different instruments and columns
The RSD values for the relative retention times of the different instruments and columns were all less than 4%, indicating good reproducibility.
The present invention also scans each component to be measured by a Diode Array Detector (DAD) to obtain the 3D absorption spectrum of each compound, as shown in fig. 1 to 4. After the peak emergence time of each component is predicted through the relative retention time, if other chromatographic peaks exist near the chromatographic peak, the positioning can be carried out according to the overall peak shape, the 3D absorption spectrogram and the like, and the method can accurately position the chromatographic peak to a certain extent by determining the relative retention time through verification.
EXAMPLE 4 sample assay accuracy study
Collecting 11 batches of Morinda officinalis medicinal materials purchased from different producing areas (see Table 4), respectively preparing test solution according to the preparation method, preparing 2 test solution in parallel for each producing area sample, carrying out sample injection measurement according to chromatographic conditions, recording the peak area of chromatographic peak of each component to be measured, and respectively adopting an external standard method (ES) and a one-test-multiple evaluation method (QAMS) to calculate the content of each component, wherein the result is shown in Table 5.
TABLE 411 Morinda officinalis sources
| Serial number | Origin of origin |
| 1 | Zhaoqing Gao Yao in Guangdong |
| 2 | Zhaoqing De Qing in Guangdong |
| 3 | Kwangdong Meizhou |
| 4 | South of Guangdong province |
| 5 | Guangxi Yulin |
| 6 | Guangxi Qinxi |
| 7 | Guangxi Qinzhou |
| 8 | Fujian Nanjing |
| 9 | Fujian Longyan |
| 10 | Hainan Qiongzhong |
| 11 | Hainan Ha |
TABLE 5 measurement results of 4 iridoid components in Morinda officinalis
Wherein, ES adopts an external standard method to determine the content of each component of the sample to be determined, QAMS is the one-measurement-multiple-evaluation method of the invention to determine the content of each component of the sample to be determined.
The ES adopts an external standard method to determine the content of each component of a sample to be detected, 4 reference substances are adopted to respectively determine the content of 4 components in the medicinal material morinda officinalis.
The data in table 5 above show that there is no significant difference in the results of the two methods, indicating that the one-test-multiple-test method established herein has high accuracy.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A quality evaluation method of morinda officinalis is characterized by comprising the following steps:
s1, preparing a mixed reference solution: preparing a mixed reference solution of the monotropein, the deacetyl asperulosidic acid, the asperulosidic acid and the asperuloside;
s2, positioning of a chromatographic peak of a component to be detected: calculating the relative retention time of each component to be detected in the mixed reference substance relative to the deacetyl asperulosidic acid by taking the deacetyl asperulosidic acid as an internal reference substance, and determining the positioning of the chromatographic peak of the component to be detected by adopting the relative retention time;
s3, calculating a relative correction factor: determining high performance liquid chromatography peaks of the components in the mixed reference substance according to the positioning of the chromatography peaks, taking deacetylated asperuloside as an internal reference substance, and respectively calculating relative correction factors of the monotropein, the asperuloside and the asperuloside according to peak areas of the chromatography peaks of the components in the mixed reference substance;
s4, sample content determination: using deacetyl asperuloside as an internal reference, determining the peak area of a chromatographic peak of a sample to be tested by using a high performance liquid phase, calculating the mass contents of the monotropein, the asperuloside and the asperuloside in morinda officinalis according to relative correction factors, establishing a multi-evaluation quality evaluation method for morinda officinalis,
wherein the conditions of the liquid chromatography are as follows: mobile phase: acetonitrile A, acetonitrile B: 0.01moL of dipotassium hydrogenphosphate + 0.2% phosphoric acid solution,
gradient elution: 0-12min, 1% A; 12-30min, 1% -A-17% A; 30-40min, 17% A;
flow rate: 1.0 mL/min-1；
Detection wavelength: 235 nm;
column temperature: 25 ℃; sample introduction amount: 20 μ L.
2. The method of claim 1, wherein the liquid chromatography column is a Venusil MP C18 column or an Agilent ZORBAX SB-Aq column, and the column size is: 250 mm. times.4.6 mm, 5 μm.
3. The method of claim 1, wherein the relative correction factor in S3 is an average of relative correction factors for mixed control solutions at 5 μ L, 10 μ L, 15 μ L, 20 μ L and 30 μ L.
4. The method of claim 3, wherein the relative correction factor for monotropein S3 is 1.3948-1.4293, the relative correction factor for asperuloside is 1.2638-1.2897, and the relative correction factor for asperuloside is 1.3152-1.3245.
5. The method of claim 4, wherein the relative correction factor for monotropein at S3 is 1.4184, the relative correction factor for asperuloside is 1.2725, and the relative correction factor for asperuloside is 1.3211.
6. The method of claim 1, wherein the relative retention time of monotropein in S2 is 0.7144-0.7483, the relative retention time of asperuloside is 2.1531-2.3162, and the relative retention time of asperuloside is 2.2926-2.4799.
7. The method of claim 9, wherein the relative retention time of monotropein in S2 is 0.7296, the relative retention time of asperuloside is 2.2179, and the relative retention time of asperuloside is 2.3858.
8. The method for evaluating the quality of Morinda officinalis according to any one of claims 1-5, wherein the method for preparing the mixed control solution in S1 comprises: add the mixed control to the initial mobile phase: acetonitrile A, acetonitrile B: dissolving 0.01moL of dipotassium hydrogen phosphate and 0.2% phosphoric acid solution and fixing the volume, wherein the mass concentration of the monotropein is 0.6352 mg/mL-1' the mass concentration of deacetyl asperuloside is 0.2100 mg/mL-1The mass concentration of the asperulosidic acid is 1.256 multiplied by 10-2mg·mL-1The mass concentration of asperuloside is 5.07 x 10-3mg·mL-1。
9. The method for assessing the quality of Morinda citrifolia according to any of claims 1 to 5, wherein the sample of S4 is prepared by the following steps: weighing morinda officinalis sample powder, adding 80% methanol solution for ultrasonic extraction, filtering to obtain filtrate, evaporating the filtrate to dryness to obtain extract residue, and mixing the extract residue with an initial mobile phase: acetonitrile A, acetonitrile B: dissolving 0.01moL of dipotassium hydrogen phosphate and 0.2% of phosphoric acid solution, metering volume to obtain an extract residue solution, and filtering to obtain a test solution.
10. The method of claim 9, wherein the ultrasound extraction time is 30min, the power is 400W, and the frequency is 90 HZ.
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