CN112834650A - Quality detection method of bone-strengthening and blood-generating oral liquid - Google Patents
Quality detection method of bone-strengthening and blood-generating oral liquid Download PDFInfo
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Abstract
The application discloses a quality detection method of bone-strengthening and blood-generating oral liquid, compared with the prior art, the quality detection method comprises the following steps: preparing a first reference substance solution; preparing a first test solution; establishing a first fingerprint of the bone-strengthening and blood-generating oral liquid; establishing standard fingerprint of the bone-strengthening and blood-generating oral liquid; preparing a second reference solution; preparing a second test solution; establishing a second fingerprint map of the bone-strengthening and blood-generating oral liquid; and comparing the second fingerprint of the bone-strengthening and blood-generating oral liquid with the standard fingerprint, and keeping the second test sample solution within +/-5% of the retention time to be qualified in detection. The application provides a quality detection method of bone-strengthening and blood-generating oral liquid, can carry out comprehensive detection to the active ingredient of bone-strengthening and blood-generating oral liquid, does benefit to the effective control to bone-strengthening and blood-generating oral liquid finished product quality to ensure the clinical curative effect of bone-strengthening and blood-generating oral liquid.
Description
Technical Field
The application relates to the field of quality detection methods, in particular to a quality detection method of an oral liquid for strengthening bone and generating blood.
Background
The oral liquid for strengthening bone and generating blood is mainly prepared from bone liquid, codonopsis pilosula, astragalus, lucid ganoderma, Chinese date, black fungus and other medicinal materials, has the functions of benefiting marrow, strengthening bone, tonifying qi and generating blood, has the functions of tonifying kidney and benefiting marrow, ensures that marrow and foot have strong bone and essence and can be converted into blood, and the bone liquid is rich in nutrient components such as calcium, so that the oral liquid for strengthening bone and generating blood can not only supplement deficiency but also prevent deficiency for the old, children and women who are pregnant and lack calcium and anemia during the lactation period, and can treat symptoms such as soreness of waist, knee weakness, weakness of feet, tooth shaking and falling, and hypoevolutism caused by deficiency, the codonopsis pilosula and the astragalus are used for tonifying qi of spleen and stomach and are used as sources of life, so that the acquired root has the origin, and qi and blood can be generated automatically, and can treat shortness of spirit, fatigue and weakness and also promote the recovery of anemia. The combination of Shen and Qin with bone fluid can nourish both spleen and kidney, so as to mutually transform bone marrow and qi and blood to nourish yin and blood. The lucid ganoderma and the Chinese date are used as ministerial drugs to strengthen the qi-tonifying effect to generate blood. Black fungus is sweet, neutral and nontoxic, and moist but not greasy, and is used as a guide to coordinate various medicines. Therefore, all the medicines are mutually matched, have mild property and taste, and tonify but not dry, have the effects of benefiting marrow, strengthening bones, tonifying qi and generating blood, and are a good prescription for treating the symptoms of marrow deficiency and bone weakness caused by calcium deficiency and anemia and deficiency of qi and blood. The oral liquid for strengthening bone and generating blood has the following clinical indications: it can be used for treating anemia and calcium deficiency of the elderly, children, and women before and after pregnancy, with the symptoms of listlessness, asthenia, pale complexion, soreness of waist and knees, muscle spasm, marasmus, odontoptosis, and infantile delayed fontanel closure, delayed teeth, delayed erection, and delayed movement.
The existing quality standard of the existing bone-strengthening and blood-generating oral liquid only measures the content of a single index component, other effective components are not monitored, certain limitation exists, and the quality level of the bone-strengthening and blood-generating oral liquid cannot be comprehensively reflected. The quality detection method for the bone-strengthening and blood-generating oral liquid is rarely disclosed, for example, Chinese patents 201210012628.4 (publication No. CN201210012628.4), 202030219270.8 (publication No. CN202030219270.8) and 202030219275.0 (publication No. CN202030219275.0) do not relate to the quality detection method; the clinical effect observation of the oral liquid for strengthening bone and generating blood in combination with the litseus sodium phosphate tablets for treating the osteoporosis of postmenopausal women in the 27 th volume and the 8 th volume of 2019 in the journal of China family planning science, the treatment effect and mechanism of the oral liquid for strengthening bone and generating blood on ovaries-removing osteoporosis rats in the 48 th volume and the 23 th volume of 2017 in the Chinese herbal medicine, the protection effect and mechanism research of the oral liquid for strengthening bone and generating blood on the bone marrow inhibition of mice after chemotherapy in the 26 th volume and the 22 th volume in the 2017 th volume in the journal of China Chinese herbal medicine, and the quality detection technology of the oral liquid for strengthening bone and generating blood in the 1 st volume in the 2004 in the Guangdong pharmacy are not related.
In the prior art, no comprehensive quality control method reflects the quality conditions of the traditional Chinese medicinal materials, intermediates and finished products, can not effectively control the production process and the product quality, and can not better ensure the clinical curative effect.
Therefore, it is a problem to be solved by those skilled in the art that how to provide a quality detection method for a bone-strengthening and blood-generating oral liquid, which can comprehensively detect the effective components of the bone-strengthening and blood-generating oral liquid.
Disclosure of Invention
In order to solve the technical problems, the application provides a quality detection method of the bone-strengthening and blood-generating oral liquid, which can comprehensively detect the effective components of the bone-strengthening and blood-generating oral liquid.
The technical scheme provided by the application is as follows:
the application provides a quality detection method of an oral liquid for strengthening bone and generating blood, which comprises the following steps: preparation of a first control solution: preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% methanol by volume percentage; preparing a first test solution: weighing 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, and taking subsequent filtrate to prepare a first test solution; a first fingerprint spectrum of the bone strengthening and blood generating oral liquid is formulated: precisely absorbing the first reference substance solution and the first test solution with the same amount respectively, injecting the first reference substance solution and the first test solution into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a first fingerprint of the bone-strengthening and blood-generating oral liquid, wherein the specific conditions of the high performance liquid chromatography are as follows: the chromatographic column is a C18 reversed phase chromatographic column; the mobile phase is gradient eluent composed of an organic phase A and a water phase B, the organic phase A is methanol or acetonitrile, and the water phase B is a formic acid solution with the volume percentage concentration of 0.1-0.4%; the detection wavelengths are 254nm, 270nm and 285nm, and the switching time of the detection wavelengths is 0min, 8min and 25 min; the column temperature is 20-40 ℃; the flow rate is 0.8mL/min to 1.2 mL/min; the analysis time is 50-65 min; gradient elution was used:
preparing a standard fingerprint spectrum of the bone-strengthening and blood-generating oral liquid: preparing a standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the bone-strengthening and blood-generating oral liquid; preparing a second reference solution; preparing a second test solution; and (3) establishing a second fingerprint of the bone-strengthening and blood-generating oral liquid: accurately sucking the second reference solution and the second test solution in equal amount respectively, injecting into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid; and comparing the second fingerprint of the bone-strengthening and blood-generating oral liquid with the standard fingerprint, and keeping the second test sample solution which is qualified in detection within +/-5 percent of the retention time.
Preferably, in the step of establishing the first fingerprint of the bone-strengthening and blood-generating oral liquid, 10 μ l of each of the first control solution and the first test solution is sucked.
Preferably, the column length of the C18 reverse phase chromatographic column is 250 mm.
Preferably, the formic acid solution has a concentration of 0.2% by volume.
Preferably, the column temperature is 30-40 ℃.
Preferably, the flow rate is 1.0 mL/min.
Preferably, the analysis time is 55 min.
Further, in a preferred mode of the present invention, the oral liquid for strengthening bone and generating blood comprises the following components in parts by weight: 600-700 parts of bone liquid, 40-50 parts of codonopsis pilosula, 70-80 parts of astragalus membranaceus, 10-20 parts of lucid ganoderma, 30-40 parts of Chinese dates and 10-20 parts of black fungus.
Further, in a preferred embodiment of the present invention, the step of "preparing the standard fingerprint of the bone-strengthening and blood-generating oral liquid" specifically comprises: and formulating the standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the 15 batches of bone-strengthening and blood-generating oral liquid.
Further, in a preferred mode of the present invention, the standard fingerprint spectrum is detected by switching wavelengths at 254nm, 270nm and 285nm, and has 12 common peaks, the sum of the areas of the common peaks accounts for more than 90% of the total peak area, the fingerprint spectrum attributed to synovial fluid has 3 common peaks, the fingerprint spectrum attributed to codonopsis pilosula has 2 common peaks, the fingerprint spectrum attributed to astragalus membranaceus has 2 common peaks, the fingerprint spectrum attributed to ganoderma lucidum has 2 common peaks, the fingerprint spectrum attributed to jujube has 2 common peaks, and the fingerprint spectrum attributed to black fungus has 1 common peak.
Further, in a preferred mode of the present invention, the standard fingerprint spectrum switches wavelengths at 254nm, 270nm and 285nm, and the retention time of the detected 12 common peaks is: (1) 5.373-5.406, (2) 5.721-5.741, (3) 6.826-6.855, (4) 8.011-8.045, (5) 9.140-9.174, (6) 10.372-10.397, (7) 11.220-11.259, (8) 14.127-14.159, (9) 16.213-16.244, (10) 18.475-18.519, (11) 19.767-19.812, and (12) 44.546-44.617.
Further, in a preferred embodiment of the present invention, the similarity between the first fingerprint of the bone-tonifying and blood-generating oral liquid and the standard fingerprint of the bone-tonifying and blood-generating oral liquid is 0.944 to 0.998.
Further, in a preferred mode of the present invention, the common peak of the first fingerprint spectrum has 11 characteristic peaks, and the retention time and relative standard deviation of each characteristic peak are as follows:
peak No. 1: retention time 5.721 ± 0.020 with relative standard deviation of 0.35%;
peak No. 2: retention time 6.826 ± 0.029 with a relative standard deviation of 0.42%;
peak No. 3: retention time 8.011 ± 0.034, relative standard deviation 0.43%;
peak No. 4: retention time 9.140 ± 0.034, relative standard deviation 0.37%;
peak No. 5: retention time 10.372 ± 0.025, relative standard deviation 0.24%;
peak No. 6: retention time 11.220 ± 0.039, relative standard deviation 0.35%;
peak No. 7: retention time 14.127 ± 0.032, relative standard deviation 0.23%;
peak No. 8: retention time 16.213 ± 0.031, relative standard deviation 0.19%;
peak No. 9: retention time 18.475 ± 0.044, relative standard deviation 0.24%;
peak No. 10: retention times 19.767 ± 0.045, relative standard deviation 0.23%;
peak No. 11: retention time 44.546 ± 0.071 with a relative standard deviation of 0.16%.
Further, in a preferred embodiment of the present invention, the step "preparing the second control solution" is the same as the step "preparing the first control solution".
Further, in a preferred mode of the present invention, the step "preparing the second sample solution" is the same as the step "preparing the first sample solution".
Further, in a preferred mode of the present invention, the specific conditions of the hplc analysis in the step of "preparing the second fingerprint of the bone-strengthening and blood-generating oral liquid" are the same as the specific conditions of the hplc analysis in the step of "preparing the first fingerprint of the bone-strengthening and blood-generating oral liquid".
Compared with the prior art, the technical scheme provided by the invention is that the quality detection method of the bone-strengthening and blood-generating oral liquid comprises the following steps: preparation of a first control solution: preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% methanol by volume percentage; preparing a first test solution: weighing 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, and taking subsequent filtrate to prepare a first test solution; a first fingerprint spectrum of the bone strengthening and blood generating oral liquid is formulated: precisely absorbing the first reference substance solution and the first test solution with the same amount respectively, injecting the first reference substance solution and the first test solution into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a first fingerprint of the bone-strengthening and blood-generating oral liquid, wherein the specific conditions of the high performance liquid chromatography are as follows: the chromatographic column is a C18 reversed phase chromatographic column; the mobile phase is gradient eluent composed of an organic phase A and a water phase B, the organic phase A is methanol or acetonitrile, and the water phase B is a formic acid solution with the volume percentage concentration of 0.1-0.4%; the detection wavelengths are 254nm, 270nm and 285nm, and the switching time of the detection wavelengths is 0min, 8min and 25 min; the column temperature is 20-40 ℃; the flow rate is 0.8mL/min to 1.2 mL/min; the analysis time is 50-65 min; gradient elution was used:
preparing a standard fingerprint spectrum of the bone-strengthening and blood-generating oral liquid: preparing a standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the bone-strengthening and blood-generating oral liquid; preparing a second reference solution; preparing a second test solution; and (3) establishing a second fingerprint of the bone-strengthening and blood-generating oral liquid: accurately sucking the second reference solution and the second test solution in equal amount respectively, injecting into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid; the second fingerprint of the bone-strengthening and blood-generating oral liquid is compared with the standard fingerprint, the qualified second test solution is reserved within +/-5% of the time, so that the components of the bone-strengthening and blood-generating oral liquid are comprehensively monitored by establishing the standard fingerprint of the bone-strengthening and blood-generating oral liquid, peak attribution and quality association of various medicinal materials of the bone-strengthening and blood-generating oral liquid and a finished product of the bone-strengthening and blood-generating oral liquid can be effectively carried out, and dynamic monitoring and tracing on the quality of a Chinese medicinal material-intermediate (sampling in the preparation process of the finished product of the bone-strengthening and blood-generating oral liquid) -finished product can be effectively carried out.
Drawings
In order to more clearly illustrate the embodiments of the present application 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 application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a standard fingerprint of a bone-strengthening and blood-generating oral liquid according to a quality detection method of the bone-strengthening and blood-generating oral liquid provided by an embodiment of the present invention;
fig. 2 is a first control solution chromatogram of a quality detection method of a bone-strengthening and blood-generating oral liquid according to an embodiment of the present invention;
fig. 3 is a full-wavelength scanning spectrum of the bone-strengthening and blood-generating oral liquid according to the quality detection method of the bone-strengthening and blood-generating oral liquid provided by the embodiment of the present invention;
fig. 4 is a first fingerprint of 15 batches of bone-strengthening and blood-generating oral liquid according to the quality detection method of the bone-strengthening and blood-generating oral liquid provided by the embodiment of the invention.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all 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 application.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or be indirectly disposed on the other element; when an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "first," "second," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, as used herein, refer to an orientation or positional relationship indicated in the drawings that is solely for the purpose of facilitating the description and simplifying the description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be considered as limiting the present application.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "plurality" or "a plurality" means two or more unless specifically limited otherwise.
It should be understood that the structures, ratios, sizes, and the like shown in the drawings are only for illustrative purposes and are not intended to limit the scope of the present disclosure, so that those skilled in the art can understand and read the present disclosure, and the present disclosure is not limited to the conditions and conditions that can be implemented in the present disclosure.
As shown in fig. 1-4, the present application provides a quality detection method of an oral liquid for strengthening bone and generating blood, comprising the following steps: preparation of a first control solution: preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% methanol by volume percentage; preparing a first test solution: weighing 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, and taking subsequent filtrate to prepare a first test solution; a first fingerprint spectrum of the bone strengthening and blood generating oral liquid is formulated: precisely absorbing the first reference substance solution and the first test solution with the same amount respectively, injecting the first reference substance solution and the first test solution into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a first fingerprint of the bone-strengthening and blood-generating oral liquid, wherein the specific conditions of the high performance liquid chromatography are as follows: the chromatographic column is a C18 reversed phase chromatographic column; the mobile phase is gradient eluent composed of an organic phase A and a water phase B, the organic phase A is methanol or acetonitrile, and the water phase B is a formic acid solution with the volume percentage concentration of 0.1-0.4%; the detection wavelengths are 254nm, 270nm and 285nm, and the switching time of the detection wavelengths is 0min, 8min and 25 min; the column temperature is 20-40 ℃; the flow rate is 0.8mL/min to 1.2 mL/min; the analysis time is 50-65 min; gradient elution was used:
preparing a standard fingerprint spectrum of the bone-strengthening and blood-generating oral liquid: preparing a standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the bone-strengthening and blood-generating oral liquid; preparing a second reference solution; preparing a second test solution; and (3) establishing a second fingerprint of the bone-strengthening and blood-generating oral liquid: accurately sucking the second reference solution and the second test solution in equal amount respectively, injecting into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid; and comparing the second fingerprint of the bone-strengthening and blood-generating oral liquid with the standard fingerprint, and keeping the second test sample solution which is qualified in detection within +/-5 percent of the retention time.
Compared with the prior art, the quality detection method of the bone-strengthening and blood-generating oral liquid comprises the following steps: preparation of a first control solution: preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% methanol by volume percentage; preparing a first test solution: weighing 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, and taking subsequent filtrate to prepare a first test solution; a first fingerprint spectrum of the bone strengthening and blood generating oral liquid is formulated: precisely absorbing the first reference substance solution and the first test solution with the same amount respectively, injecting the first reference substance solution and the first test solution into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a first fingerprint of the bone-strengthening and blood-generating oral liquid, wherein the specific conditions of the high performance liquid chromatography are as follows: the chromatographic column is a C18 reversed phase chromatographic column; the mobile phase is gradient eluent composed of an organic phase A and a water phase B, the organic phase A is methanol or acetonitrile, and the water phase B is a formic acid solution with the volume percentage concentration of 0.1-0.4%; the detection wavelengths are 254nm, 270nm and 285nm, and the switching time of the detection wavelengths is 0min, 8min and 25 min; the column temperature is 20-40 ℃; the flow rate is 0.8mL/min to 1.2 mL/min; the analysis time is 50-65 min; gradient elution was used:
preparing a standard fingerprint spectrum of the bone-strengthening and blood-generating oral liquid: preparing a standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the bone-strengthening and blood-generating oral liquid; preparing a second reference solution; preparing a second test solution; and (3) establishing a second fingerprint of the bone-strengthening and blood-generating oral liquid: accurately sucking the second reference solution and the second test solution in equal amount respectively, injecting into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid; the second fingerprint of the bone-strengthening and blood-generating oral liquid is compared with the standard fingerprint, the qualified second test solution is reserved within +/-5% of the time, so that the components of the bone-strengthening and blood-generating oral liquid are comprehensively monitored by establishing the standard fingerprint of the bone-strengthening and blood-generating oral liquid, peak attribution and quality association of various medicinal materials of the bone-strengthening and blood-generating oral liquid and a finished product of the bone-strengthening and blood-generating oral liquid can be effectively carried out, and dynamic monitoring and tracing on the quality of a Chinese medicinal material-intermediate (sampling in the preparation process of the finished product of the bone-strengthening and blood-generating oral liquid) -finished product can be effectively carried out.
It should be added that, in the embodiment of the present invention, the hplc analysis employs three wavelengths with detection wavelengths of 254nm, 270nm, and 285nm, determines the maximum absorption wavelength of each component of the bone-strengthening and blood-generating oral liquid by full-wavelength scanning, and then determines the detection wavelengths in different intervals according to the spectrum absorption of the specific component, so that the quality monitoring of each component in the bone-strengthening and blood-generating oral liquid can be more accurately performed, the purpose of increasing the quality coverage can be achieved by using the interval segmented wavelength detection method, the detection quality and the detection sensitivity can be effectively improved, the quality of the bone-strengthening and blood-generating oral liquid can be comprehensively, objectively, and scientifically evaluated, and the method can be used as an important basis for identifying the authenticity of the bone-strengthening and blood-generating oral liquid.
Specifically, in the embodiment of the invention, the oral liquid for strengthening bone and generating blood comprises the following components in parts by weight: 600-700 parts of bone liquid, 40-50 parts of codonopsis pilosula, 70-80 parts of astragalus membranaceus, 10-20 parts of lucid ganoderma, 30-40 parts of Chinese dates and 10-20 parts of black fungus.
Specifically, in the embodiment of the present invention, the step of "preparing the standard fingerprint of the bone-strengthening and blood-generating oral liquid" specifically comprises: and formulating the standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the 15 batches of bone-strengthening and blood-generating oral liquid.
Specifically, in the embodiment of the invention, the standard fingerprint spectrum is detected by switching wavelengths under 254nm, 270nm and 285nm, and has 12 common peaks, the sum of the peak areas of the common peaks accounts for more than 90% of the total peak area, the fingerprint spectrum attributed to bone fluid has 3 common peaks, the fingerprint spectrum attributed to codonopsis pilosula has 2 common peaks, the fingerprint spectrum attributed to astragalus membranaceus has 2 common peaks, the fingerprint spectrum attributed to ganoderma lucidum has 2 common peaks, the fingerprint spectrum attributed to jujube has 2 common peaks, the fingerprint spectrum attributed to black fungus has 1 common peak, the established standard fingerprint spectrum has 12 common peaks, the information content is large, and chemical components in the test solution can be completely reserved.
Specifically, in the embodiment of the present invention, the standard fingerprint spectrum switches wavelengths at 254nm, 270nm, and 285nm, and the retention times of the detected 12 common peaks are: (1) 5.373-5.406, (2) 5.721-5.741, (3) 6.826-6.855, (4) 8.011-8.045, (5) 9.140-9.174, (6) 10.372-10.397, (7) 11.220-11.259, (8) 14.127-14.159, (9) 16.213-16.244, (10) 18.475-18.519, (11) 19.767-19.812, and (12) 44.546-44.617.
It should be added that, in the present embodiment, the retention time of the common peak is calculated by using the bone-strengthening and blood-generating oral liquid with the batch number of 2006021 as the reference map S1.
Specifically, in the embodiment of the invention, the similarity between the first fingerprint of the bone-strengthening and blood-generating oral liquid and the standard fingerprint of the bone-strengthening and blood-generating oral liquid is 0.944-0.998.
It should be added that, in the embodiment of the present invention, a standard feature map is prepared by using traditional Chinese medicine fingerprint similarity evaluation software according to a first feature map determined by 15 batches of common peaks of the first fingerprint of the bone-strengthening and blood-generating oral liquid, where the standard feature map has 11 feature peaks, the bone-strengthening and blood-generating oral liquid with the batch number of 2006021 is used as a reference map S1, and retention time and relative standard deviation of each feature peak are as follows:
peak No. 1: retention time 5.721 ± 0.020 with relative standard deviation of 0.35%;
peak No. 2: retention time 6.826 ± 0.029 with a relative standard deviation of 0.42%;
peak No. 3: retention time 8.011 ± 0.034, relative standard deviation 0.43%;
peak No. 4: retention time 9.140 ± 0.034, relative standard deviation 0.37%;
peak No. 5: retention time 10.372 ± 0.025, relative standard deviation 0.24%;
peak No. 6: retention time 11.220 ± 0.039, relative standard deviation 0.35%;
peak No. 7: retention time 14.127 ± 0.032, relative standard deviation 0.23%;
peak No. 8: retention time 16.213 ± 0.031, relative standard deviation 0.19%;
peak No. 9: retention time 18.475 ± 0.044, relative standard deviation 0.24%;
peak No. 10: retention times 19.767 ± 0.045, relative standard deviation 0.23%;
peak No. 11: retention time 44.546 ± 0.071 with a relative standard deviation of 0.16%.
More specifically, the preferred retention time of each peak in the standard fingerprint is as follows: (1) 5.340-5.406, (2) 5.701-5.741, (3) 6.797-6.855, (4) 7.977-8.045, (5) 9.106-9.174, (6) 10.347-10.397, (7) 11.181-11.259, (8) 14.095-14.159, (9) 16.182-16.244, (10) 18.431-18.519, (11) 19.722-19.812, and (12) 44.475-44.617.
Specifically, in the present example, the step "preparing the second control solution" is the same as the step "preparing the first control solution".
More specifically, the "preparing the second control solution" is specifically: the calycosin glucoside is prepared into a second reference solution containing 0.001-0.004 mg of calycosin glucoside per 1mL by using 50-100% methanol by volume percentage.
Specifically, in the present embodiment, the step "preparing the second sample solution" is the same as the step "preparing the first sample solution".
More specifically, the "preparing the second sample solution" specifically includes: taking 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, taking the subsequent filtrate, and preparing a second test solution.
Specifically, in the embodiment of the present invention, the specific conditions of the hplc analysis in the step of "preparing the second fingerprint of the bone-strengthening and blood-generating oral liquid" are the same as the specific conditions of the hplc analysis in the step of "preparing the first fingerprint of the bone-strengthening and blood-generating oral liquid".
It should be added that, in the embodiment of the present invention, through traditional Chinese medicine fingerprint similarity evaluation software, a second feature spectrum is determined according to a common peak of a second fingerprint of the bone-strengthening and blood-generating oral liquid of 15 batches, the second feature spectrum is compared with the standard fingerprint, and the second test solution that is qualified in detection is determined when the retention time is within ± 5%.
The quality detection method of the bone-strengthening and blood-generating oral liquid provided by the invention comprises the following specific operation steps or working principle:
preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% of methanol, measuring 5mL of bone-tonifying oral liquid, putting the bone-tonifying oral liquid into a 50mL volumetric flask, adding 0-50% of methanol or 0-50% of ethanol to 50mL scale positions, shaking uniformly, filtering by using a microporous membrane, taking subsequent filtrate to prepare a first sample solution, respectively and precisely absorbing the first reference solution and the first sample solution in equal amount, injecting the first sample solution and the first sample solution into a liquid chromatograph for high performance liquid chromatography analysis, determining to obtain a first fingerprint of the bone-tonifying oral liquid, formulating a standard fingerprint of the bone-tonifying oral liquid according to the first fingerprint of the bone-tonifying oral liquid, preparing a second reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% of methanol, measuring 5mL of the bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, taking a subsequent filtrate to prepare a second test solution, respectively and precisely absorbing the second reference solution and the second test solution in equal amount, injecting the solution into a liquid chromatograph for high performance liquid chromatography analysis, determining to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid, comparing the second fingerprint of the bone-strengthening and blood-generating oral liquid with a standard fingerprint, retaining the qualified second test solution within +/-5% of the time, determining a second characteristic map according to the common peak of the second fingerprint of the bone-strengthening and blood-generating oral liquid in 15 batches by traditional Chinese medicine fingerprint similarity evaluation software, comparing the second characteristic map with the standard fingerprint, the second test solution qualified for detection is reserved within +/-5%, the high performance liquid chromatography fingerprint detection method provided by the invention has the advantages of higher precision, better stability, shorter analysis time and certain specificity, the separation degree of each characteristic peak in the detected fingerprint is better, the fingerprint of the bone-strengthening and blood-generating oral liquid and the fingerprint of the intermediate of the bone-strengthening and blood-generating oral liquid have better correlation, the application of the intermediate of the bone-strengthening and blood-generating oral liquid and the finished product fingerprint thereof can enhance the quality controllability in the production process, the application of the fingerprint of the bone-strengthening and blood-generating oral liquid can comprehensively reflect whether the production process is uniform and stable, and the quality stability and the clinical curative effect of the bone-strengthening and blood-generating oral liquid can be ensured.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A quality detection method of an oral liquid for strengthening bone and generating blood is characterized by comprising the following steps:
preparation of a first control solution: preparing the calycosin glucoside into a first reference solution containing 0.001-0.004 mg of the calycosin glucoside per 1mL by using 50-100% methanol by volume percentage;
preparing a first test solution: weighing 5mL of bone-strengthening and blood-generating oral liquid, placing the oral liquid in a 50mL volumetric flask, adding 0-50% methanol or 0-50% ethanol to 50mL scale positions, shaking up, filtering with a microporous membrane, and taking subsequent filtrate to prepare a first test solution;
a first fingerprint spectrum of the bone strengthening and blood generating oral liquid is formulated: precisely absorbing the first reference substance solution and the first test solution with the same amount respectively, injecting the first reference substance solution and the first test solution into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a first fingerprint of the bone-strengthening and blood-generating oral liquid, wherein the specific conditions of the high performance liquid chromatography are as follows: the chromatographic column is a C18 reversed phase chromatographic column; the mobile phase is gradient eluent composed of an organic phase A and a water phase B, the organic phase A is methanol or acetonitrile, and the water phase B is a formic acid solution with the volume percentage concentration of 0.1-0.4%; the detection wavelengths are 254nm, 270nm and 285nm, and the switching time of the detection wavelengths is 0min, 8min and 25 min; the column temperature is 20-40 ℃; the flow rate is 0.8mL/min to 1.2 mL/min; the analysis time is 50-65 min; gradient elution was used:
preparing a standard fingerprint spectrum of the bone-strengthening and blood-generating oral liquid: preparing a standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the bone-strengthening and blood-generating oral liquid;
preparing a second reference solution;
preparing a second test solution;
and (3) establishing a second fingerprint of the bone-strengthening and blood-generating oral liquid: accurately sucking the second reference solution and the second test solution in equal amount respectively, injecting into a liquid chromatograph for high performance liquid chromatography, and measuring to obtain a second fingerprint of the bone-strengthening and blood-generating oral liquid;
and comparing the second fingerprint of the bone-strengthening and blood-generating oral liquid with the standard fingerprint, and keeping the second test sample solution which is qualified in detection within +/-5 percent of the retention time.
2. The quality detection method of the oral liquid for bone-strengthening and blood-generating according to claim 1, wherein the oral liquid for bone-strengthening and blood-generating comprises the following components in parts by weight: 600-700 parts of bone liquid, 40-50 parts of codonopsis pilosula, 70-80 parts of astragalus membranaceus, 10-20 parts of lucid ganoderma, 30-40 parts of Chinese dates and 10-20 parts of black fungus.
3. The method for detecting the quality of the oral liquid for strengthening bone and generating blood according to claim 2, wherein the step of establishing the standard fingerprint of the oral liquid for strengthening bone and generating blood specifically comprises the following steps: and formulating the standard fingerprint of the bone-strengthening and blood-generating oral liquid according to the first fingerprint of the 15 batches of bone-strengthening and blood-generating oral liquid.
4. The method for detecting the quality of the oral liquid for strengthening bone and generating blood according to claim 3, wherein the standard fingerprint spectrum is detected by switching wavelengths under 254nm, 270nm and 285nm, and has 12 common peaks, the sum of the areas of the common peaks accounts for more than 90% of the total peak area, the fingerprint spectrum attributed to the bone liquid has 3 common peaks, the fingerprint spectrum attributed to codonopsis pilosula has 2 common peaks, the fingerprint spectrum attributed to astragalus has 2 common peaks, the fingerprint spectrum attributed to ganoderma has 2 common peaks, the fingerprint spectrum attributed to jujube has 2 common peaks, and the fingerprint spectrum attributed to black fungus has 1 common peak.
5. The method for detecting the quality of oral liquid for bone strengthening and blood generation according to claim 4, wherein the standard fingerprint spectrum switches wavelengths at 254nm, 270nm and 285nm, and the retention time of the detected 12 common peaks is as follows: (1) 5.373-5.406, (2) 5.721-5.741, (3) 6.826-6.855, (4) 8.011-8.045, (5) 9.140-9.174, (6) 10.372-10.397, (7) 11.220-11.259, (8) 14.127-14.159, (9) 16.213-16.244, (10) 18.475-18.519, (11) 19.767-19.812, and (12) 44.546-44.617.
6. The method for detecting the quality of the oral liquid for bone-strengthening and blood-generating as claimed in claim 5, wherein the similarity between the first fingerprint of the oral liquid for bone-strengthening and blood-generating and the standard fingerprint of the oral liquid for bone-strengthening and blood-generating is 0.944-0.998.
7. The method for detecting the quality of oral liquid for bone-strengthening and blood-generating according to claim 6, wherein the common peaks of the first fingerprint have 11 characteristic peaks, and the retention time and the relative standard deviation of each characteristic peak are as follows:
peak No. 1: retention time 5.721 ± 0.020 with relative standard deviation of 0.35%;
peak No. 2: retention time 6.826 ± 0.029 with a relative standard deviation of 0.42%;
peak No. 3: retention time 8.011 ± 0.034, relative standard deviation 0.43%;
peak No. 4: retention time 9.140 ± 0.034, relative standard deviation 0.37%;
peak No. 5: retention time 10.372 ± 0.025, relative standard deviation 0.24%;
peak No. 6: retention time 11.220 ± 0.039, relative standard deviation 0.35%;
peak No. 7: retention time 14.127 ± 0.032, relative standard deviation 0.23%;
peak No. 8: retention time 16.213 ± 0.031, relative standard deviation 0.19%;
peak No. 9: retention time 18.475 ± 0.044, relative standard deviation 0.24%;
peak No. 10: retention times 19.767 ± 0.045, relative standard deviation 0.23%;
peak No. 11: retention time 44.546 ± 0.071 with a relative standard deviation of 0.16%.
8. The method for detecting the quality of oral liquid for bone strengthening and hematogenesis as claimed in claim 7, wherein the step of preparing the second control solution is the same as the step of preparing the first control solution.
9. The method for detecting the quality of oral liquid for bone strengthening and blood generation as claimed in claim 8, wherein the step of preparing the second sample solution is the same as the step of preparing the first sample solution.
10. The method for detecting the quality of an oral liquid for enriching the bone and generating blood as claimed in claim 9, wherein the specific conditions of the hplc analysis for preparing the second fingerprint of the oral liquid for enriching the bone and generating blood in the step "are the same as the specific conditions of the hplc analysis for preparing the first fingerprint of the oral liquid for enriching the bone and generating blood in the step" are the same.
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