CN106706825B - Method for determining content of tetrahydropalmatine in bergamot Rupining - Google Patents

Method for determining content of tetrahydropalmatine in bergamot Rupining Download PDF

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CN106706825B
CN106706825B CN201510788686.XA CN201510788686A CN106706825B CN 106706825 B CN106706825 B CN 106706825B CN 201510788686 A CN201510788686 A CN 201510788686A CN 106706825 B CN106706825 B CN 106706825B
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周桂荣
耿婉丽
霍志鹏
何毅
周水平
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Tasly Pharmaceutical Group Co Ltd
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    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract

The invention relates to a method for measuring the content of tetrahydropalmatine in bergamot rupi ning, which comprises the following steps: step 1, preparing a reference substance solution, step 2, preparing a test solution, step 3, injecting the reference substance solution and the test solution into a high performance liquid chromatograph to obtain a chromatogram, and step 4, calculating the content of tetrahydropalmatine in the test solution according to the chromatogram.

Description

Method for determining content of tetrahydropalmatine in bergamot Rupining
The technical field is as follows:
the invention relates to a detection method of active ingredients in a medicament, in particular to a content determination method of tetrahydropalmatine in bergamot rupi ning.
Background art:
the tangerine peel capsule for treating mammary gland hyperplasia is a traditional Chinese medicine preparation for soothing liver, regulating qi, relieving pain, activating blood, resolving masses and regulating menstruation and is used for treating mammary gland hyperplasia caused by liver depression, qi stagnation and phlegm coagulation stasis, and is prepared from traditional Chinese medicinal materials such as rhizoma cyperi, tangerine leaves, selfheal, salvia miltiorrhiza, rhizoma bolbostemmae, corydalis tuber, Chinese rose flowers and the like at the present research stage. Wherein rhizoma cyperi is taken as a monarch drug and orange leaves are taken as ministerial drugs.
The preparation method of the tangerine peel capsules for treating mammary nodule disease comprises the following steps: decocting folium Citri Gangerinae, Prunellae Spica and flos Rosae chinensis with 12 times of water for 3 times, each time for 1 hr, mixing decoctions, filtering, concentrating the filtrate under reduced pressure to obtain fluid extract with relative density of 1.08-1.10(60 deg.C), adding ethanol to make ethanol content reach 70%, standing overnight, collecting supernatant, concentrating under reduced pressure to obtain soft extract with relative density of 1.28-1.30(60 deg.C), and drying under reduced pressure; extracting rhizoma Cyperi, Saviae Miltiorrhizae radix, rhizoma Bolbostematis, and rhizoma corydalis with 70% ethanol for 3 times (7 times for the first time and 6 times for the second and third times respectively for 1.5 hr), mixing extractive solutions, filtering, concentrating the filtrate under reduced pressure to obtain soft extract with relative density of 1.28-1.30(60 deg.C), drying under reduced pressure, mixing with the above water extraction and ethanol precipitation dry extract, pulverizing into fine powder, mixing the dry extract powder with appropriate amount of starch and microcrystalline cellulose, granulating, adding magnesium stearate and silica gel, mixing, encapsulating, and packaging with aluminum plastic.
Tetrahydropalmatine is the main component of rhizoma corydalis, and is the index component in quality control of XIANGJUSHUANNING Capsule. The method for determining the content of tetrahydropalmatine in the bergamot Rupining capsule adopts acetonitrile-0.1% phosphoric acid (pH is adjusted to 7.0 by triethylamine) (40:60) as a mobile phase, and the column temperature is 30 ℃, however, the existing method has many defects, such as: the separation degree of target components is sensitive to pH value, the repeatability of prepared mobile phase is poor, the base line of a sample is seriously drifted and deformed after continuous sample injection, a column is easy to block after continuous sample injection of a plurality of needles, the column pressure is increased, and the like.
The invention content is as follows:
in order to solve the problems, the invention optimizes the tetrahydropalmatine content determination method on the basis of the original tetrahydropalmatine content determination method, and the optimized tetrahydropalmatine content determination method specifically comprises the following steps:
a method for measuring the content of tetrahydropalmatine in bergamot Rupining comprises the following steps:
step 1, preparing a reference substance solution,
step 2, preparing a test solution,
step 3, injecting the reference solution and the sample solution into a high performance liquid chromatograph to obtain a chromatogram,
step 4, calculating the content of tetrahydropalmatine in the test sample according to the chromatogram,
wherein the chromatographic conditions are as follows:
wherein the number of theoretical plates is not less than 3000 calculated according to tetrahydropalmatine peak. The chromatographic column adopts octadecylsilane chemically bonded silica as a filler, the mobile phase is acetonitrile-triethylamine aqueous solution, wherein the volume ratio of triethylamine in the aqueous phase is 0.01-0.03%, the detection wavelength is 265-295nm, and the column temperature is 25-45 ℃. The detection wavelength was 280 nm. The column temperature was 35 ℃. The gradient elution procedure was as follows:
Figure BDA0000848967270000021
wherein the preparation method of the reference substance solution in the step 1 comprises the following steps:
adding methanol into tetrahydropalmatine control, and making into solution containing 5-20 μ g per 1 ml. Preferably, the method is as follows: weighing appropriate amount of tetrahydropalmatine reference substance, and adding methanol to obtain solution containing 10 μ g per 1 ml.
Wherein the preparation method of the test solution in the step 2 comprises the following steps: grinding the sample, adding 0.1-1g diluted ethanol 5-20ml, ultrasonic treating for more than 15min, cooling, adding diluted ethanol, diluting, and filtering to obtain filtrate. Preferably, the method is as follows: grinding the content of the product, precisely weighing about 0.3g, placing in a 10ml measuring flask, adding diluted ethanol about 8ml, ultrasonic treating for 15min (120W, 40KHz), cooling, adding diluted ethanol to dilute to scale, shaking, filtering, and collecting the filtrate.
The method of the step 3 comprises the following steps: injecting 5-20 μ l of reference solution and 5-20 μ l of test solution into liquid chromatograph to obtain chromatogram, and calculating tetrahydropalmatine content by using external standard two-point method logarithmic equation. The preferred method is as follows: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
The chromatographic conditions of the method are obtained by screening:
1. selection of measurement wavelength
By performing ultraviolet scanning on tetrahydropalmatine reference solution, the maximum absorption peak at 282nm is obtained, and 280nm is selected as detection wavelength by referring to the original method.
2. Selection of mobile phase
In the original method, acetonitrile-0.1% phosphoric acid (pH is adjusted to 7.0 by triethylamine) is adopted as a mobile phase, the ratio of the acetonitrile to the phosphoric acid is 40:60, however, the separation degree of a target component is sensitive to the pH value, the repeatability of the prepared mobile phase is poor, the separation degree is not good, and a shoulder appears. See fig. 1.
In order to solve the problem, according to the property of tetrahydropalmatine, in order to avoid the tailing of the peak shape, an alkaline mobile phase condition is selected, through investigation and comparison, 0.02 percent of triethylamine water is selected as a water phase, the peak shape is good, the tailing is not generated, the forward extension is not generated, when the concentration of triethylamine is respectively 0.01 percent, 0.02 percent and 0.03 percent, the peak shape is good, the mobile phase is simple to prepare and easy to operate, so that the acetonitrile-0.02 percent of triethylamine water is selected as the mobile phase. Chromatogram is shown in FIG. 2
3 solution preparation method
The preparation method of the reference substance and the test substance is the same as the original method, and the original method selects the optimal parameters by researching the extraction solvent, the extraction time and the purification method, so that the new method selects the solution preparation method which is the same as the original method.
4 methodological investigation
4.1 specificity test
Precisely measuring blank solvent, rhizoma corydalis deficiency negative solution, tetrahydropalmatine reference solution, and test solution 10 μ l each, injecting into liquid chromatograph, and recording liquid chromatogram. As can be known from a liquid chromatogram, the baseline separation of the tetrahydropalmatine and other components can be achieved under the chromatographic condition, no absorption peak appears on the position of the rhizoma corydalis-deficient negative sample corresponding to the tetrahydropalmatine reference, and the number of theoretical plates is not less than 3000 calculated according to the tetrahydropalmatine peak. The results are shown in FIGS. 3, 4, 5 and 6.
4.2 instrumental precision test
The control solutions with concentrations of 2.39. mu.g/ml, 11.97. mu.g/ml and 35.90. mu.g/ml were taken, 10. mu.l of the control solution was precisely aspirated, and the results were continuously measured 6 times, as shown in Table 2.
TABLE 2 results of precision test
Figure BDA0000848967270000031
Figure BDA0000848967270000041
The test result shows that: the precision of the instrument is good under high, medium and low concentrations.
4.3 Linear
Accurately weighing 11.98mg of tetrahydropalmatine reference substance, placing in a 100ml measuring flask, adding methanol to dissolve and dilute to scale, and shaking to obtain 119.8 μ g/ml reference substance solution (mother liquor). The mother liquor was diluted as follows:
1ml→50ml；1ml→25ml；2ml→25ml；1ml→10ml；3ml→25ml；3ml→10ml
each 10. mu.l of the solution was precisely aspirated, and the solution was injected into a liquid chromatograph and measured. The results of linear regression by the least square method using the peak area (A) as the ordinate (Y) and the amount of sample (. mu.g) as the abscissa (X) are shown in Table 3 and FIG. 7.
TABLE 3 examination of the Linear relationship
Figure BDA0000848967270000042
The test result shows that: the sample amount of the tetrahydropalmatine reference substance is in the range of 0.0239-0.359 mu g, and the sample amount (mu g) and the peak area form a good linear relation.
4.4 repeatability test
Grinding the contents of the product (lot 20131004) with different contents, weighing 6 parts, each part is about 0.3g, precisely weighing, placing in 10ml volumetric flask, adding diluted ethanol about 8ml, ultrasonic treating for 15min, cooling, adding diluted ethanol to scale, shaking, filtering, and collecting the filtrate. Precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and measuring to obtain the results shown in Table 4.
TABLE 4 results of the repeatability tests
Figure BDA0000848967270000051
The test result shows that: the coefficient of variation RSD of the content of 6 samples is 1.90 percent, which indicates that the method has good repeatability.
4.5 intermediate precision
Replacing the instrument, grinding the content of the product (batch No. 20131004) with different loading amount, weighing 6 parts, each part is about 0.3g, accurately weighing, placing in 10ml volumetric flask, adding diluted ethanol about 8ml, ultrasonic treating for 15min, cooling, adding diluted ethanol to scale, shaking, filtering, and collecting the filtrate. Precisely sucking 10 μ l of each of the control solution and the sample solution, injecting into a liquid chromatograph, and measuring to obtain the results shown in Table 5.
TABLE 5 results of intermediate precision test
Figure BDA0000848967270000052
The test result shows that: the coefficient of variation RSD of the content of 6 samples was 0.89%, and the average value was 0.0221mg/g and RSD was 4.17% when 6 measurements of intermediate precision and 6 measurements of reproducibility were combined.
4.6 recovery test
Taking 6 parts of a test sample (batch No. 20131004, the content is 0.023mg/g according to the average value of a repeatability test) with known content, each part is about 0.15g, precisely weighing, placing the test sample into a 10ml volumetric flask, precisely adding 1ml of tetrahydropalmatine reference substance with the concentration of 35.90 mu g/m, respectively, preparing 6 parts of test sample solution according to the preparation method of the test sample solution, precisely sucking 10 mu l of each of the reference sample solution and the test sample solution, injecting the test sample solution into a liquid chromatograph, and measuring, wherein the results are shown in Table 7.
Figure BDA0000848967270000061
TABLE 6 recovery test results
Figure BDA0000848967270000062
The test result shows that: the method has good recovery rate.
4.7 durability test
In order to investigate the durability of the method, factors such as temperature, detection wavelength, flow rate, chromatographic column, triethylamine concentration, mobile phase ratio and the like are fluctuated in a small range, content measurement is carried out on the same sample, and RSD of each experimental content measurement result is taken as an investigation index to investigate the content. The results and the analysis thereof are shown in tables 7 and 8, respectively.
TABLE 7 durability examination results
Figure BDA0000848967270000063
Figure BDA0000848967270000071
From the above experimental results, we can generalize and analyze it to obtain the following analysis results:
TABLE 8 analysis of durability examination results
Figure BDA0000848967270000072
The results of the above table and the spectrograms show that the separation degree is not affected when each typical variable factor of the method is changed in a small range, the RSD value of each factor is larger when each factor is changed due to lower content, the RSD of other variable factors except the column temperature is less than 5%, and the RSD is 8.44% when the column temperature is changed at the upper and lower 5 ℃ within an acceptable range, which indicates that the column temperature has larger influence on the measurement result and needs to be noticed in the measurement process. The column temperature is set to 35 ℃ because at higher temperature, the adsorption of sample components in the chromatographic column is less, more sample components are washed off, and the phenomenon that the chromatographic column is blocked and the pressure is increased rapidly after the chromatographic column is used for a period of time is avoided.
4.8 method comparison
The contents of this product (lot 20131004) were ground to fine powder, and 2 parts (about 0.3g each) were weighed and subjected to content measurement by the original method and the new method, respectively, and the results are shown in Table 9.
TABLE 9 comparison of the methods
Figure BDA0000848967270000081
The test result shows that: both methods agree on the measurement results.
5. Summary of the invention
Through verification, the new method can be used for measuring the tetrahydropalmatine content in the bergamot Rupining capsules, and is superior to the original method in durability and convenient operation. And the problems that the separation degree is sensitive to the pH value, the separation degree is reduced when the pH value is slightly changed, the base line drifts and deforms after continuous sample injection, the column is easy to block, the column pressure is easy to rise and the like in the original method are solved.
Description of the drawings:
FIG. 1 original method chromatogram
FIG. 2 chromatogram of the method of the invention
FIG. 3 blank solvent
Figure 4 rhizoma corydalis deficiency negativity
Figure 5 tetrahydropalmatine control solution
FIG. 6 control solution
FIG. 7 Linearity of tetrahydropalmatine content determination method
The specific implementation mode is as follows:
the invention is further illustrated by the following examples.
Example 1
(1) The instrument comprises the following steps: waters e2695 hplc; waters Empower Pro workstation, Waters2998 model ultraviolet detector.
(2) Reagent and reagent
Tetrahydropalmatine control: provided by the institute of Chinese food and drug testing, for content determination, batch number: 110726-201414. Methanol and acetonitrile are used as chromatographic purities, ethanol, phosphoric acid and triethylamine are used as analytical purities, and water is fresh deionized water.
(3) Chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.02% triethylamine water as mobile phase, gradient elution is shown in table 1; the detection wavelength is 280nm, and the column temperature is 35 ℃. The number of theoretical plates is not less than 3000 calculated according to tetrahydropalmatine peak.
Table 1: gradient of mobile phase
Figure BDA0000848967270000091
Example 2
(1) Waters e2695 hplc; waters Empower Pro workstation, Waters 2489 model ultraviolet detector.
(2) Reagent and reagent
Tetrahydropalmatine control: provided by the institute of Chinese food and drug testing, for content determination, batch number: 110726-201414. Methanol and acetonitrile are used as chromatographic purities, ethanol, phosphoric acid and triethylamine are used as analytical purities, and water is fresh deionized water.
(3) Chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.01% triethylamine water as mobile phase, gradient elution is shown in table 1; the detection wavelength is 265nm and the column temperature is 25 ℃. The number of theoretical plates is not less than 3000 calculated according to tetrahydropalmatine peak.
Table 1: gradient of mobile phase
Figure BDA0000848967270000092
Example 3
(1) Waters e2695 hplc; waters Empower Pro workstation, Waters 2489 model ultraviolet detector.
(2) Reagent and reagent
Tetrahydropalmatine control: provided by the institute of Chinese food and drug testing, for content determination, batch number: 110726-201414. Methanol and acetonitrile are used as chromatographic purities, ethanol, phosphoric acid and triethylamine are used as analytical purities, and water is fresh deionized water.
(3) Chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.03% triethylamine water as mobile phase, gradient elution is shown in table 1; the detection wavelength is 295nm, and the column temperature is 45 ℃. The number of theoretical plates is not less than 3000 calculated according to tetrahydropalmatine peak.
Table 1: gradient of mobile phase
Figure BDA0000848967270000101

Claims (5)

1. A method for measuring the content of tetrahydropalmatine in bergamot Rupining comprises the following steps:
step 1, preparing a reference substance solution,
step 2, preparing a test solution,
step 3, injecting the reference solution and the sample solution into a high performance liquid chromatograph to obtain a chromatogram,
step 4, calculating the content of tetrahydropalmatine in the test sample according to the chromatogram,
wherein, the preparation method of the reference substance solution in the step 1 comprises the following steps: adding methanol into tetrahydropalmatine control to obtain solution containing 5-20 μ g per 1 ml;
wherein, the preparation method of the test solution in the step 2 comprises the following steps: grinding the sample, adding 0.1-1g of diluted ethanol 5-20ml, ultrasonic treating for more than 15min, cooling, diluting with diluted ethanol, and filtering to obtain filtrate;
wherein, the chromatographic conditions are as follows:
the number of theoretical plates is not less than 3000 calculated according to tetrahydropalmatine peak, the chromatographic column adopts octadecylsilane chemically bonded silica as filler, the mobile phase is acetonitrile-triethylamine aqueous solution, wherein the volume ratio of triethylamine in the aqueous phase is 0.01-0.03%, gradient elution is adopted, the detection wavelength is 280nm, the column temperature is 35 ℃,
the gradient elution procedure was as follows:
Figure FDA0002250927660000011
。
2. the method of claim 1, wherein said control solution is prepared in step 1 by: adding methanol into tetrahydropalmatine control, and making into solution containing 10 μ g per 1 ml.
3. The method of claim 1, wherein said sample solution is prepared in step 2 by: grinding the sample, collecting 0.3g, precisely weighing, placing in 10ml measuring flask, adding diluted ethanol 8ml, ultrasonic treating for 15min, cooling, adding diluted ethanol to dilute to scale, shaking, filtering, and collecting the filtrate.
4. The method of claim 1, wherein the method of step 3 is as follows: injecting 5-20 μ l of reference solution and 5-20 μ l of test solution into liquid chromatograph to obtain chromatogram, and calculating tetrahydropalmatine content by external standard point method.
5. The method according to claim 1, characterized by the steps of:
wherein the preparation method of the reference substance solution in the step 1 comprises the following steps: weighing appropriate amount of tetrahydropalmatine reference substance, and adding methanol to obtain solution containing 10 μ g per 1 ml;
wherein the preparation method of the test solution in the step 2 comprises the following steps: taking a sample, grinding, taking 0.3g, precisely weighing, placing in a 10ml measuring flask, adding diluted ethanol about 8ml, ultrasonically treating for 15 minutes, cooling, adding diluted ethanol to dilute to scale, shaking up, filtering, and taking a subsequent filtrate to obtain the final product;
the method of the step 3 comprises the following steps: respectively sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and measuring;
wherein, the chromatographic conditions are as follows:
the instrument adopts a Waters e2695 high performance liquid chromatograph; waters Empower Pro workstation, Waters2998 type ultraviolet detector, the chromatographic conditions are: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.02% triethylamine water as mobile phase, gradient elution; the detection wavelength is 280nm, the column temperature is 35 ℃, the number of theoretical plates is not less than 3000 calculated according to the tetrahydropalmatine peak,
gradient elution procedure
Figure FDA0002250927660000021
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CN104415573A (en) * 2013-09-10 2015-03-18 中国科学院大连化学物理研究所 Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract

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Title
RP-HPLC法测定痛经宝颗粒中延胡索乙素的含量;杨晓秋 等;《医药产业资讯》;20060731;第3卷(第20期);第138-139页 *

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