CN112505173B - Method for measuring synephrine content in dried orange peel - Google Patents
Method for measuring synephrine content in dried orange peel Download PDFInfo
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Abstract
The invention belongs to the field of pharmaceutical chemicals, and relates to a method for measuring the content of synephrine in pericarpium citri reticulatae. The method can quickly and accurately detect the synephrine content in the dried orange peel.
Description
The application is filed on 7/1/2015, has the application number of 201510381434.5, and is a divisional application named as a method for detecting the stability of the process of the warm gall bladder tablets.
Technical Field
The invention belongs to the field of pharmaceutical chemicals, and relates to a method for measuring synephrine content in dried orange peel.
Background
The gallbladder warming tablet is a medicine developed in the traditional Chinese medicine pharmacy of the first subsidiary hospital of Guangzhou Chinese medicine university, which is approved as the No. 98 Hospital A-294 of the Tiaowei medical (province) in 1998 and can treat vertigo, emesis, vexation, insomnia, palpitation, epilepsy and other diseases.
The preparation method of WENDAN tablet comprises mixing radix Curcumae, rhizoma Pinelliae Preparata, fructus Aurantii Immaturus, pericarpium Citri Tangerinae, glycyrrhrizae radix, caulis Bambusae in Taenia and Poria, sequentially extracting with solvent, concentrating, precipitating with ethanol and refining. Because the process steps of the lining warming tablet are multiple and the related components are complex, no method for detecting the quality stability or the process stability exists at present, and the quality or the process of the lining warming tablet cannot be controlled.
Synephrine is an adrenoceptor stimulant, has the effects of improving metabolism, increasing calorie consumption and oxidizing fat, is widely applied to the industries of medicine, food, beverage and the like, and is named as 4- [ 1-hydroxy-2- (methylamino) ethyl ] phenol by IUPAC (international association of pharmaceutical and food products), and has the following structural formula:
disclosure of Invention
The traditional Chinese medicine preparation gallbladder warming tablet has various medicinal materials, complex components and complicated process links, and a method for detecting the process stability is not available at present. The inventor of the invention surprisingly finds that the process stability of the warming-in-container tablet can be detected by measuring the synephrine transfer rate of the warming-in-container tablet, thereby well controlling the product quality stability of the warming-in-container tablet.
The seven medicinal materials for producing the gallbladder warming tablet of the invention have the following proportions: 400-800 parts of bamboo shavings, 400-700 parts of rhizoma pinellinae praeparata, 400-700 parts of radix curcumae, 100-300 parts of liquorice, 100-300 parts of dried orange peel, 400-800 parts of poria cocos and 400-800 parts of immature bitter orange.
The traditional Chinese medicine composition is prepared from 550-750 parts by weight of bamboo shavings, 450-600 parts by weight of rhizoma pinellinae praeparata, 450-600 parts by weight of radix curcumae, 150-250 parts by weight of liquorice, 150-250 parts by weight of dried orange peel, 450-600 parts by weight of poria cocos and 550-750 parts by weight of immature bitter orange.
Preferably, 660 parts of caulis bambusae in taeniam, 550 parts of rhizoma pinellinae praeparata, 550 parts of radix curcumae, 165 parts of liquorice, 165 parts of dried orange peel, 550 parts of poria cocos and 660 parts of immature bitter orange. Or 500 parts of caulis bambusae in taeniam, 450 parts of rhizoma pinellinae praeparata, 500 parts of radix curcumae, 150 parts of liquorice, 200 parts of pericarpium citri reticulatae, 600 parts of poria cocos and 700 parts of immature bitter orange.
The preparation method of the gallbladder warming tablet comprises the following steps: mixing radix Curcumae, rhizoma Pinelliae Preparata, fructus Aurantii Immaturus, pericarpium Citri Tangerinae, glycyrrhrizae radix, caulis Bambusae in Taenia and Poria at above ratio, soaking in water for half an hour, heating to boil, reflux-extracting for 1-2h, extracting twice, condensing during extraction to collect volatile oil, filtering the extractive solution, concentrating, precipitating with ethanol, filtering, concentrating the supernatant to obtain soft extract, adding adjuvants to make into granule, spraying volatile oil, and tabletting. The collected volatile oil contains the components of the raw medicinal materials and is also an effective component for exerting the drug effect.
The gallbladder warming tablet is produced by seven medicinal materials, wherein the content determination and the chemical component research of rhizoma pinellinae praeparata, radix curcumae, caulis bambusae in taeniam and poria cocos are not related in pharmacopoeia of the people's republic of china (2010 edition). Only the literature can be found that rhizoma Pinelliae Preparata contains trigonelline, radix Curcumae contains curcumin, and caulis Bambusae in Taenia contains tricin.
The inventor researches the three components and the raw medicinal materials and finds that: when the medicinal material curcuma aromatica is curcuma wenyujin, the curcuma aromatica does not contain curcumin; the content of the tricin in the bamboo shavings is only 0.0087%, and the content is too low to be detected easily; in addition to rhizoma Pinelliae Preparata, radix Glycyrrhizae also contains trigonelline and has a content higher than that of rhizoma Pinelliae Preparata, and has poor specificity of trigonelline component, and radix Glycyrrhizae is a messenger drug and its component is not suitable as index; accordingly, none of the above three components is suitable as a detection index.
The inventor carries out intensive research on two medicinal materials of the tangerine peel and the immature bitter orange, and finds that the tangerine peel and the immature bitter orange both contain hesperidin and synephrine, and the chemical components of the tangerine peel and the immature bitter orange are close. The inventor researches the quality stability and the process stability of the warming gallbladder tablets by taking hesperidin and synephrine as detection indexes respectively, and finds that the transfer rate of the hesperidin is too low in the process of preparing the warming gallbladder tablets, so that the detection is easy to cause inaccuracy and is not suitable for serving as the index, and the synephrine transfer rate is higher and is suitable for serving as the detection index.
The invention relates to a method for detecting the process stability of a lining warming tablet, which comprises the step of measuring the synephrine transfer rate of the lining warming tablet.
In one embodiment of the method of the invention, when the synephrine transfer rate is more than or equal to 40.8%, the process stability is qualified; specifically, when the synephrine transfer rate is more than or equal to 41%, more than or equal to 42%, more than or equal to 43.5%, more than or equal to 44%, more than or equal to 45.4%, more than or equal to 46%, more than or equal to 47%, more than or equal to 48%, more than or equal to 49%, more than or equal to 50%, or more than or equal to 50.21%, the process stability is qualified.
In any embodiment of the methods of the invention, the synephrine transfer rate =100% x synephrine mass in fel tablet (μ g)/synephrine mass in drug (μ g).
In one embodiment of any of the methods of the invention, the amount of synephrine in the botanical is (μ g) = the amount of synephrine in the prescribed citrus aurantium (μ g) + the amount of synephrine in the prescribed citrus peel (μ g); specifically, the mass (μ g) of synephrine in the prescription immature bitter orange is not less than the mass (g) of the prescription immature bitter orange and the synephrine content (μ g/g) in the prescription immature bitter orange; specifically, the mass (μ g) of synephrine in the prescription pericarpium citri reticulatae is not less than the mass (g) of the prescription pericarpium citri reticulatae and the synephrine content (μ g/g) in the prescription pericarpium citri reticulatae.
In an embodiment of any of the methods of the invention, the determination of synephrine content in prescription immature bitter orange is performed according to pharmacopoeia of the people's republic of china (2010 edition), p 230; specifically, the method for measuring the content of synephrine in the tangerine peel comprises the steps of mixing the tangerine peel and methanol, and measuring the content of the synephrine in an extracting solution by liquid chromatography.
In any embodiment of the methods of the invention, the determination of the synephrine content of citrus peel comprises any one or more of the following (1) to (4),
(1) Before mixing, crushing the dried orange peel into medium powder;
(2) Adding 50-100mL of methanol into per gram of dried orange peel;
(3) Mixing under ultrasound; specifically, after ultrasonic treatment, methanol is used for complementing loss weight loss;
(4) Filtering the extractive solution; specifically, the filter pore size is 0.22. Mu.m.
In any embodiment of the method of the present invention, the liquid chromatography detection conditions for measuring the content of citrus peel synephrine are any one or more of the following (1) to (7),
(1) The chromatographic column is a normal phase silica gel bonded diol-based chromatographic column;
(2) The detection wavelength is 275nm;
(3) The flow rate of the mobile phase is 0.6-1.2mL/min;
(4) The theoretical plate number is greater than or equal to 14000;
(5) The liquid chromatography is high performance liquid chromatography;
(6) Column temperature: 35 ℃;
(7) The mobile phase A is 5mM ammonium acetate solution, the mobile phase B is acetonitrile, the volume percentage changes of the mobile phases A and B are shown in the following table,
in any embodiment of the method of the present invention, the quality measurement of synephrine in the Winterian tablets comprises the steps of mixing the Winterian tablets with methanol and measuring the content of synephrine in the extract by liquid chromatography.
In any embodiment of the methods of the invention, the Wencandine synephrine assay comprises any one or more of the following (1) to (5),
(1) Before mixing, crushing the warm gall pieces;
(2) Mixing under ultrasound; specifically, after ultrasonic treatment, methanol is used for complementing loss weight loss;
(3) Methanol concentration of 50-100% v/v;
(4) Adding 50-100mL of methanol into each gram of gallbladder warming tablets;
(5) Filtering the extractive solution; specifically, the filtrate is further purified; the preferred purification step is evaporation of the filtrate to dryness-dissolution of the residue-elution through a polyamide column.
In any embodiment of the method of the present invention, the conditions for the liquid chromatography detection of the content of the Chondrus crispus are any one or more of the following (1) to (6),
(1) The chromatographic column is a normal phase silica gel bonded diol-based chromatographic column;
(2) Acetonitrile and ammonium acetate solution are used as mobile phases; preferably, acetonitrile is used as the mobile phase A, and 5mmol/L ammonium acetate solution is used as the mobile phase B; more preferably, the volume ratio of mobile phase a to mobile phase B is (60-95): (5-40);
(3) The detection wavelength is 275nm;
(4) The flow rate of the mobile phase is 0.6-1.2mL/min;
(5) The theoretical plate number is more than or equal to 14000;
(6) The liquid chromatography is high performance liquid chromatography.
In the present invention, the term "process stability" refers to the ability of the process to withstand fluctuations in materials and process and equipment changes without negative quality impact (ICH process robustness).
In the present invention, the term "medium powder" means powder which can pass through the sieve No. four in its entirety, but mixed with powder which can pass through the sieve No. five by not more than 60%.
In the present invention, the term "theoretical plate number" refers to one of column efficiency parameters of chromatography, which is used to quantitatively express the separation efficiency of a chromatography column.
Advantageous effects of the invention
(1) The stability of the gallbladder warming tablet process is detected by the synephrine transfer rate value of the gallbladder warming tablet.
(2) The invention further takes the synephrine transfer rate of the warming gallbladder tablets to be more than or equal to 40.8 percent as the qualified standard of the process stability of the warming gallbladder tablets, thereby realizing the control of the product quality of the warming gallbladder tablets.
(3) The liquid chromatography detection of the invention uses the normal phase silica gel bonded diol-based chromatographic column, which can better retain the synephrine component, and has the advantages of shorter equilibrium time, higher determination speed, higher sensitivity and higher separation degree.
In addition, the normal phase silica gel bonded diol-based chromatographic column does not need to be added with an ion pair reagent, so that the damage to the chromatographic column is reduced, and the synephrine component can be better retained on the chromatographic column.
(4) The sample extraction method is simple, the impurity content of the sample is low, the interference on a liquid chromatograph is reduced, and the detection accuracy is improved.
Drawings
FIG. 1: the invention adopts acetonitrile with the volume ratio of 80 to 20 and 5mmol/L ammonium acetate solution as mobile phase to detect the liquid chromatogram of the content of synephrine in the Wendan tablet I.
FIG. 2: the invention adopts acetonitrile with the volume ratio of 90 to 10 and 5mmol/L ammonium acetate solution as mobile phase to detect the liquid chromatogram of the content of synephrine in the Wendan tablet I.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are commercially available, and are not indicated by manufacturers.
1. Preparation of warming gallbladder tablet
Preparation example 1
Mixing 660 parts of seven medicinal materials including bamboo shavings, 550 parts of rhizoma pinellinae praeparata, 550 parts of radix curcumae, 165 parts of liquorice, 165 parts of dried orange peel, 550 parts of poria cocos and 660 parts of immature bitter orange in proportion, adding water to soak for half an hour, heating to boil, performing reflux extraction for 1.5 hours, extracting twice, condensing and collecting volatile oil in the extraction process, filtering the extracting solution, concentrating at 80 ℃, performing ethanol precipitation and filtration, concentrating the supernatant into thick paste at 80 ℃, adding dextrin to prepare granules, spraying the volatile oil, and tabletting to obtain the first batch of gallbladder warming tablets.
Preparation example 2
Mixing 550 parts by weight of seven medicinal materials of bamboo shavings, 450 parts by weight of rhizoma pinellinae praeparata, 450 parts by weight of radix curcumae, 150 parts by weight of liquorice, 150 parts by weight of dried orange peel, 450 parts by weight of poria cocos and 550 parts by weight of immature bitter orange in proportion, adding water for soaking for half an hour, heating to boil, performing reflux extraction for 1.5h, extracting twice, collecting volatile oil in the extraction process, filtering the extracting solution, concentrating at 80 ℃, performing ethanol precipitation and filtration, concentrating the supernatant into thick paste at 80 ℃, adding dextrin to prepare granules, spraying the volatile oil, and tabletting to obtain the second batch of the gallbladder warming tablets.
Preparation example 3
Mixing 750 parts by weight of seven medicinal materials of bamboo shavings, 600 parts by weight of rhizoma pinellinae praeparata, 600 parts by weight of radix curcumae, 250 parts by weight of liquorice, 250 parts by weight of dried orange peel, 600 parts by weight of poria cocos and 700 parts by weight of immature bitter orange in proportion, adding water for soaking for half an hour, heating to boil, performing reflux extraction for 1.5h, extracting twice, collecting volatile oil in the extraction process, filtering the extracting solution, concentrating at 80 ℃, performing ethanol precipitation and filtration, concentrating the supernatant into thick paste at 80 ℃, adding dextrin to prepare granules, spraying the volatile oil, and tabletting to obtain the third batch of gallbladder warming tablets.
2. Method for measuring synephrine transfer rate and hesperidin transfer rate of Wendan tablets
The synephrine standard and the hesperidin standard used for determination are provided by China food and drug testing research institute, and the batch numbers are 110727-201107 and 110721-201115 respectively.
Method for measuring synephrine transfer rate of Wendan tablet
(1) Quality determination of synephrine in Wendan tablet
(1) Extracting a sample by a lining:
taking 10 warm gallbladder tablets (about 0.25 g/tablet) per batch, crushing, grinding into fine powder, weighing 1g of the warm gallbladder tablet fine powder, adding 50-100mL of 50-100% (v/v) methanol, weighing, carrying out ultrasonic treatment for 10-60min, cooling to room temperature, weighing again, supplementing the lost weight with 50-100% (v/v) methanol, cooling, filtering, precisely weighing 10mL of subsequent filtrate, evaporating to dryness, dissolving 10mL of residue in water, loading the residue into a column by a dry method through polyamide (60-90 meshes, 2.5g, with the inner diameter of 1 cm), eluting with 25mL of water, collecting the eluate, transferring to a 25mL volumetric flask, adding water to the scale, and shaking uniformly to obtain the product;
(2) determination of synephrine content of sample:
detecting the sample by high performance liquid chromatography (Shimadzu LC-20AT high performance liquid chromatograph; SPD-M20A ultraviolet detector; labsolutions data processing software system) under the following chromatographic conditions: sample injection amount: 10 mul; and (3) chromatographic column: normal phase silica gel bonded Diol-based chromatography column (YMC-Pack Diol-120-NP, 250X 4.6mm,5 μm,12 nm); mobile phase: acetonitrile is used as a mobile phase A,5mmol/L ammonium acetate solution is used as a mobile phase B, and the volume ratio of the mobile phase A to the mobile phase B is 80:20; the detection wavelength is 275nm, the flow rate is 1.0mL/min, and the number of theoretical plates is not less than 14000.
(3) The method for calculating the synephrine mass in the Wendan tablets comprises the following steps:
and (2) adding water into the synephrine standard substance to respectively prepare 7 standard solutions of 7.44 mu g/mL, 14.88 mu g/mL, 29.76 mu g/mL, 59.52 mu g/mL, 89.28 mu g/mL, 119.04 mu g/mL and 148.8 mu g/mL, detecting the 7 standard solutions according to the method, carrying out linear regression by taking the concentration of the standard solutions as an abscissa and the chromatographic peak area as an ordinate to obtain a linear equation y =5218.2x-1829.9, R =0.9999, substituting the chromatographic peak area of the sample into the linear equation to calculate the synephrine content of the sample, and calculating the synephrine mass in the wenchong tablet according to the following formula.
Quality of synephrine (μ g) = synephrine content of sample (μ g/mL) × 25mL × dilution times × quality of each batch of fel warming tablets (g)/quality of fel warming tablet fine powder (g)
Wherein dilution factor = initial added methanol volume (mL)/10 mL.
(2) The quality of synephrine in the medicinal materials is determined:
in the formula I, both the immature bitter orange and the dried orange peel contain synephrine, the synephrine content in the immature bitter orange in the formula is determined according to pages 230-231 of pharmacopoeia of the people's republic of China (2010 edition), and page number difference can be caused due to different printing batches.
II, measuring the content of synephrine in the tangerine peel with the prescription:
i. extracting a sample from dried orange peel:
precisely weighing 3 parts (used for calculating the average value) of the dried orange peel medium powder, wherein each part is about 1g, respectively placing the dried orange peel medium powder into 200mL conical bottles with stoppers, precisely adding 100mL of methanol, weighing, and ultrasonically treating for 1h. Weighing, adding methanol to complement weight loss, shaking, and filtering with 0.22 μm microporous membrane.
A sample detection method:
reference is made to the synephrine plasmid assay in Wendan tablets (2).
The difference lies in that: column temperature: 35 ℃; mobile phase a was 5mM ammonium acetate solution, mobile phase B was acetonitrile, and the volume percent changes of mobile phase a, B are shown in table 1.
TABLE 1
A calculation method:
dissolving synephrine standard with chromatographic pure methanol to obtain standard solution with synephrine content of 0.036mg/ml, and measuring the standard solution according to the above method. Calculating by adopting an external standard method to obtain the synephrine content of the sample, and calculating according to the following formula to obtain the synephrine content in the tangerine peel of the prescription.
The content of synephrine in the tangerine peel of the prescription (mug/g) = the content of synephrine in a sample (mug/mL) × 100 mL/tangerine peel medium powder mass (g)
III, calculating according to the following formula to obtain the quality of the synephrine in the medicinal materials.
The mass of synephrine in the medicinal materials (mug) = the mass of prescription immature bitter orange (g) × synephrine content in prescription immature bitter orange (mug/g) + the mass of prescription dried orange peel (g) × synephrine content in prescription dried orange peel (mug/g)
(3) Calculating the synephrine transfer rate of the Wendan tablets:
the synephrine transfer rate of the Wendan tablets is calculated according to the following formula.
Synephrine transfer rate =100% × synephrine mass in wendan tablet (μ g)/synephrine mass in medicinal material (μ g)
Method for measuring hesperidin transfer rate of (II) wendan tablets
(1) Measuring the quality of hesperidin in the gallbladder warming tablet:
(1) extracting a sample from a gallbladder warming sheet:
grinding fel Ursi in mortar, precisely weighing 0.5g, placing in conical flask with plug, precisely adding 50mL methanol, sealing, weighing, ultrasonic treating (power 250W, frequency 59 kHz) for 30min, cooling, weighing again, supplementing the weight loss with methanol, shaking, filtering, and collecting the filtrate.
(2) Measuring the content of hesperidin in a sample:
detecting a sample by using high performance liquid chromatography, wherein the chromatographic conditions are as follows: sample introduction amount: 10 mul; octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.1% phosphoric acid (volume ratio 20: 80) is used as a mobile phase; the detection wavelength is 285nm; column temperature: 35 ℃; the theoretical plate number is not less than 15000 in terms of hesperidin peak.
(3) The method for calculating the content of hesperidin in the gallbladder warming tablet comprises the following steps:
taking a proper amount of hesperidin standard, dissolving with pure water to prepare a standard solution of 0.11mg/mL, detecting the standard solution according to the method, and calculating the hesperidin quality in the gallbladder warming tablet by adopting an external standard method and according to the following formula.
The quality = V sample, A sample, C standard, m batch/(A standard, m sample) of hesperidin in the gallbladder warming tablet
Wherein, the V sample is the total volume (mL) of the sample, the A sample is the peak area of the sample, the C standard is the concentration (mu g/mL) of the standard solution, the A standard is the peak area of the standard solution, the m sample is the sampling quantity (g) of the lining plate, and the m batches are the mass (g) of the lining plate of each batch.
(2) The quality of hesperidin in the medicinal materials is determined:
the immature bitter orange and the tangerine peel in the prescription contain hesperidin, the content of the hesperidin in the tangerine peel in the prescription is determined according to pages 176-177 of pharmacopoeia of the people's republic of China (2010 version), and page numbers can be different due to different printing batches.
II, measuring the content of hesperidin in the immature bitter orange in the prescription:
i. extracting a sample from immature bitter orange:
in reference to (one), 2. Ii. I, a sample is extracted from dried orange peel. Except that the immature bitter orange middle powder is used for replacing the dried orange peel middle powder.
A sample detection method:
and detecting the sample by using high performance liquid chromatography. The chromatographic conditions are as follows: sample introduction amount: 10 mu L of the solution; and (3) chromatographic column: YMC-Pack, ODS-AM, 4.6X 250mm,5 μm; a detector: an ultraviolet detector; detection wavelength: 283nm; column temperature: 35 ℃; flow rate: 1.0mL/min; mobile phase A: water, mobile phase B acetonitrile, and the volume ratio of A to B is 80:20.
a method of calculation:
dissolving hesperidin standard with chromatographic pure methanol to obtain standard solution with hesperidin content of 0.080mg/mL, and detecting the standard solution according to the above method. And calculating to obtain the hesperidin content of the sample by adopting an external standard method, and calculating to obtain the hesperidin content in the immature bitter orange in the formula by referring to the step (I) - (2), the step (II) and the step (iii).
III, calculating the mass of the hesperidin in the medicinal materials according to the following formula.
The weight (mug) of hesperidin in the medicinal materials is not less than the weight (g) of prescription immature bitter orange multiplied by the content (mug/g) of hesperidin in prescription immature bitter orange, the weight (g) of prescription dried orange peel multiplied by the content (mug/g) of hesperidin in prescription dried orange peel
(3) Calculating the hesperidin transfer rate of the swertia mileensis tablet:
the transfer rate of the hesperidin in the gallbladder warming tablet is calculated according to the following formula.
Hesperidin transfer rate =100% × hesperidin quality in fel warming tablet (μ g)/hesperidin quality in medicinal material (μ g)
3. Evaluation of Process stability
The synephrine transfer rate and the hesperidin transfer rate were measured in accordance with the second procedure using the Wendan tablets of batches I, II and III of preparation examples 1 to 3, respectively, and the results are shown in Table 2.
TABLE 2
As can be seen from Table 2, the synephrine transfer rate in the production of the warming gallbladder tablets is far greater than the hesperidin transfer rate, and the synephrine transfer rate is easier to measure accurately and is suitable for being used as an index for evaluating the process stability. Moreover, the synephrine transfer rate of the preparation examples 1-3 is more than or equal to 40.8%, which indicates that the preparation process of the fel warming tablets of the preparation examples 1-3 has high stability.
In addition, 10 batches of the warming gallbladder tablets were prepared according to preparation examples 1 to 3, respectively, and 10 batches produced according to preparation example 1 were named warming gallbladder tablets I1 to I10, 10 batches produced according to preparation example 2 were named warming gallbladder tablets II 1 to II 10, and 10 batches produced according to preparation example 3 were named warming gallbladder tablets III 1 to III 10. Measuring the synephrine transfer rate of each batch of gallbladder-warming tablets according to the second method, and the result shows that the synephrine transfer rate of the gallbladder-warming tablets I1 to I10 is close to 50.68 percent; the synephrine transfer rate of the warming gallbladder tablets II 1-II 10 is close to 51.94 percent; the synephrine transfer rate of the warming gallbladder tablets III 1-III 10 is close to 50.21%. The synephrine transfer rate is more than or equal to 40.8 percent, and the preparation process of the gallbladder warming tablet is stable.
In addition, when measuring the synephrine mass in the Wendan tablet I, the sample detection is carried out by respectively adopting two mobile phases A and B with the volume ratio of 80 and 90.
As can be seen from comparison of fig. 1 and fig. 2, the volume ratio of mobile phase a to B is 80.
4. Methodology research for detecting stability of warming-gallbladder sheet process
(1) Precision:
the prepared synephrine standard solution with the concentration of 29.76 mu g/mL is measured according to the method in the second.
(2) Stability:
the sample is extracted from the Winterepha I according to the method in the second (first) to the method in the first (1), the sample is measured for 5 times, 10 mu l of the sample is injected into the high performance liquid chromatography at the time points of the beginning, 6h, 12h, 24h and 36h respectively, the synephrine chromatographic peak area is measured, the RSD of the chromatographic peak area is calculated for 5 times to be 1.85, and the result shows that the extracted sample is stable within 36 hours.
(3) Reproducibility:
6 parts of samples of the swertia mileensis I are prepared and measured according to the method in the second (first) to (1), and the RSD of the content of synephrine in the swertia mileensis is 1.92, which indicates that the method has good reproducibility.
(4) Sample recovery rate:
crushing and grinding 10 pieces of fel warming tablets I (the measured synephrine content is 3.80 mg/g) into fine powder, weighing 6 parts of fel warming tablets 0.5g, respectively adding synephrine standard substance of about 1.9mg into a bottle with a corkscrew, respectively measuring the synephrine content of the added standard substance by a two.
Sample recovery rate = (sample adding synephrine content-Wendan I synephrine content)/standard sample adding amount × 100%
As a result, the average value of the sample recovery rate of synephrine is 97.6%, the RSD is 0.96%, and the sample recovery rate meets the requirement, which shows that the method has higher accuracy.
Although specific embodiments of the invention have been described in detail, those skilled in the art will appreciate. Various modifications and substitutions of those details may be made in light of the overall teachings of the disclosure, and such changes are intended to be within the scope of the present invention. The full scope of the invention is given by the appended claims and any equivalents thereof.
Claims (4)
1. A method for measuring the content of synephrine in dried orange peel is characterized by comprising the steps of mixing dried orange peel and methanol, and measuring the content of synephrine in an extracting solution by liquid chromatography;
the detection conditions of the liquid chromatogram are as follows:
(1) The chromatographic column is a normal phase silica gel bonded diol-based chromatographic column;
(2) The detection wavelength is 275nm;
(3) The flow rate of the mobile phase is 0.6-1.2mL/min;
(4) The theoretical plate number is more than or equal to 14000;
(5) The liquid chromatography is high performance liquid chromatography;
(6) Column temperature: 35 ℃;
(7) The mobile phase A is 5mM ammonium acetate solution, the mobile phase B is acetonitrile, and the volume percentage changes of the mobile phases A and B are as follows:
2. the method of claim 1, comprising any one or more of the following (1) - (4):
(1) Before mixing, crushing the dried orange peel into medium powder;
(2) Adding 50-100mL of methanol into per gram of dried orange peel;
(3) Mixing under ultrasound;
(4) Filtering the extractive solution.
3. The method according to claim 2, wherein in the step (3), the loss and weight loss amount is made up with methanol after the sonication.
4. The method according to claim 2, wherein in the step (4), the pore size of the filter membrane is 0.22 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011272381.0A CN112505173B (en) | 2015-07-01 | 2015-07-01 | Method for measuring synephrine content in dried orange peel |
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| CN201510381434.5A CN106323794B (en) | 2015-07-01 | 2015-07-01 | Method for detecting process stability of gallbladder warming tablets |
| CN202011272381.0A CN112505173B (en) | 2015-07-01 | 2015-07-01 | Method for measuring synephrine content in dried orange peel |
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| CN201510381434.5A Division CN106323794B (en) | 2015-07-01 | 2015-07-01 | Method for detecting process stability of gallbladder warming tablets |
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Effective date of registration: 20230524 Address after: 363000 No. 1, Amber Road, Xiangcheng District, Zhangzhou City, Fujian Province Patentee after: ZHANGZHOU PIEN TZE HUANG PHARMACEUTICAL Co.,Ltd. Address before: 510405 No.16 Airport Road, Baiyun District, Guangzhou City, Guangdong Province Patentee before: The First Affiliated Hospital of Guangzhou University of Chinese Medicine |