CN1758058A - Determination method of naringoside content in stomach intestine calm pill - Google Patents
Determination method of naringoside content in stomach intestine calm pill Download PDFInfo
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- CN1758058A CN1758058A CN 200510014880 CN200510014880A CN1758058A CN 1758058 A CN1758058 A CN 1758058A CN 200510014880 CN200510014880 CN 200510014880 CN 200510014880 A CN200510014880 A CN 200510014880A CN 1758058 A CN1758058 A CN 1758058A
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Abstract
This invention discloses a method for testing the content of shaddock skin glycoside in the stomach safety pills including the following steps: 1, preparing a check sample solution: taking suitable volume of shaddock skin glycoside to be added with methyl alcohol to finish a check sample solution, 2, preparing a sample solution: taking the stomach safety pill to be grinded, taking the powder and putting it in a conical flask to be added with the methyl alcohol to be heated in water bath then flowing back to be cooled and weighed accurately to be filtered by a micro-hole film to be prepare for test, 3, testing it with a high efficient liquid phase chromatograph.
Description
Technical field
The present invention relates to the assay method of naringin content in a kind of Chinese medicine preparation, particularly relate to a kind of assay method that utilizes naringin content in the high effective liquid chromatography for measuring Chinese medicine preparation gastrointestinal disease treating pill.
Background technology
At present, along with the continuous development of the modernization of Chinese medicine, the improving constantly of pharmaceutical technology (tcd) and quality testing level, increasing advanced detecting instrument and laboratory facilities are used to the detection of Chinese patent drug quality.Simultaneously, along with the raising of people's living standard, society is also more and more higher to the quality requirements of medicine, and this will have advanced person, stable, reliable detection method that the quality of medicine is effectively controlled with regard to requiring each pharmacy corporation.Therefore, the quality standard of raising Chinese patent drug is imperative.
In addition, country encourages each pharmacy corporation and R﹠D institution to improve existing Chinese patent drug quality standard, and passes through the raising that some approach promote quality standards, for example:
1.2005 " Chinese pharmacopoeia has increased qualitative, the quantitative identification method of many Chinese crude drugs and Chinese patent drug to a year version on the basis of version in 2000;
2. in the process that medicine registrations such as new product development and old product secondary development are declared, all require on the basis of initial quality standard, to improve.
Gastrointestinal disease treating pill be in the pure Chinese medicinal preparation of the treatment enterogastric diseases developed of new medicine company Lerentang Traditional Chinese Medicine Factory, Tianjin, record in " Chinese pharmacopoeia version in 2000, this prescription is made up of flavour of a drug such as the banksia rose, agalloch eaglewood, rheum officinale, Fructus Aurantiis, have eliminate dampness with aromatics, regulating qi-flowing for relieving pain has to be good for the stomach and leads stagnant merit, clinically is used for the treatment of diseases such as diarrhoea, enteritis, bacillary dysentery, gastral cavity abdomen overflow, stomachache and dyspepsia breast that indigestion causes be long-pending.Fructus Aurantii is main flavour of a drug in the prescription, plays the gas of sharp chest abdomen, the long-pending ruffian that disappears of loosing, dampness elimination and leads stagnant helping digestion.Aurantiin is one of principal ingredient in the Fructus Aurantii, and higher because of aurantiin content in the Fructus Aurantii medicinal material, therefore and stable in properties, can control this product inherent quality effectively by the monitoring to naringin content in the gastrointestinal disease treating pill.
Summary of the invention
The assay method that the purpose of this invention is to provide naringin content in a kind of gastrointestinal disease treating pill, the present invention is the content that utilizes aurantiin in the high effective liquid chromatography for measuring gastrointestinal disease treating pill, to improve the quality standard of gastrointestinal disease treating pill.
Technical scheme of the present invention is summarized as follows:
The assay method of naringin content in a kind of gastrointestinal disease treating pill, form by following steps:
(1) it is an amount of that the aurantiin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 0.0119mg/ml～0.119mg/ml, preferably 0.01mg/ml, product solution in contrast;
(2) the gastrointestinal disease treating pill porphyrize is got in the preparation of need testing solution, and it is fixed to get the accurate title of powder 0.1g, puts 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decided water-bath reflux 20-90 minute, preferably 30 minutes, put and be chilled to room temperature, the accurate title, decide, and supplies with methyl alcohol to subtract weight loss, and miillpore filter filters, as need testing solution, the miillpore filter aperture is 0.45 μ m preferably;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and 0.1%～1% glacial acetic acid aqueous solution is 10～50: 90～50, and best the concentration of described glacial acetic acid aqueous solution is concentration of volume percent than being 20: 80, and preferred concentration is 0.3%; Detect wavelength: 217nm; Flow velocity: 0.5ml/min～1.0ml/min, optimum flow rate are 0.8ml/min; 20 ℃～40 ℃ of column temperatures are advisable with 35 ℃, and precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measure.
Advantage of the present invention is: easily and fast, specificity and favorable reproducibility, the result can be used for the quality control of gastrointestinal disease treating pill accurately and reliably.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of reference substance aurantiin;
Fig. 2 is the high-efficient liquid phase chromatogram of aurantiin in the gastrointestinal disease treating pill;
The high-efficient liquid phase chromatogram of the negative reference substance of Fig. 3.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
The assay method of naringin content comprises the steps: in a kind of gastrointestinal disease treating pill
(1) it is an amount of that the aurantiin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 0.01mg/ml, in contrast product solution;
(2) the gastrointestinal disease treating pill porphyrize is got in the preparation of need testing solution, it is fixed to get the accurate title of powder 0.1g, put 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, water-bath reflux 30 minutes, put and be chilled to room temperature, the accurate title, decide, and supplies with methyl alcohol to subtract weight loss, 0.45 μ m miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and 0.3% glacial acetic acid aqueous solution is 20: 80, and the concentration of described glacial acetic acid aqueous solution is concentration of volume percent; Detect wavelength: 217nm; Flow velocity: 0.8ml/min; 35 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 2
The assay method of naringin content comprises the steps: in a kind of gastrointestinal disease treating pill
(1) it is an amount of that the aurantiin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 0.0119mg/ml, in contrast product solution;
(2) the gastrointestinal disease treating pill porphyrize is got in the preparation of need testing solution, and it is fixed to get the accurate title of powder 0.1g, puts 50ml tool plug conical flask, adds methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 20 minutes is put and is chilled to room temperature, and accurate title is fixed, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and 0.1% glacial acetic acid aqueous solution is 50: 50, and the concentration of described glacial acetic acid aqueous solution is concentration of volume percent; Detect wavelength: 217nm; Flow velocity: 0.5ml/min; 20 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 3
The assay method of naringin content comprises the steps: in a kind of gastrointestinal disease treating pill
(1) it is an amount of that the aurantiin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 0.119mg/ml, in contrast product solution;
(2) the gastrointestinal disease treating pill porphyrize is got in the preparation of need testing solution, and it is fixed to get the accurate title of powder 0.1g, puts 50ml tool plug conical flask, adds methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 90 minutes is put and is chilled to room temperature, and accurate title is fixed, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and 1% glacial acetic acid aqueous solution is 10: 90, and the concentration of described glacial acetic acid aqueous solution is concentration of volume percent; Detect wavelength: 217nm; Flow velocity: 1.0ml/min; 40 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 4
Accurate aurantiin reference substance solution (concentration is 0.0119mg/ml) 2,4,8,12,16, the 20 μ l sample introductions of drawing of the investigation of linear relationship, measure by above-mentioned chromatographic condition, sample size with the aurantiin reference substance is a horizontal ordinate, respective peaks area integral value is an ordinate, the calculating regression equation is Y=4666857X-15551.9, r=0.99995 (r: related coefficient).The aurantiin reference substance solution becomes good linear relationship in 0.0119～0.119mg/ml scope.
Embodiment 5
Same need testing solution is got in the precision experiment, and continuous 6 sample introductions record the peak area integrated value, and RSD (relative standard deviation) is 1.7% as a result.
Embodiment 6
Same batch sample is got in the reappearance experiment, takes by weighing 6 parts of test samples, according to need testing solution preparation method preparation, measures content, and average content is 11.38mg/g, and RSD is 1.45%, shows that this law reappearance is good, and precision is higher.
Embodiment 7
Stability experiment is got same need testing solution, and every 2 hours sample introduction 2 μ l, sample introduction was 6 times altogether, measures peak area and calculates content, and RSD is 1.7% (n=6) as a result.
Embodiment 8
The application of sample absorption method is adopted in recovery experiment, gets 6 parts in the sample of known content (11.38mg/g), accurately respectively adds a certain amount of aurantiin reference substance, measures according to content assaying method, calculates average recovery, the results are shown in Table 1.
Table 1. recovery test result
Table 1 Result of recovery test
| Sample volume (g) | Sample naringin content (mg) | Aurantiin addition (mg) | Measurement result (mg) | The recovery (%) | Average recovery rate (%) | RSD (％) |
| 0.0531 0.0543 0.0535 0.0533 0.0545 0.0473 | 0.6037 0.6181 0.6091 0.6071 0.6205 0.5378 | 0.5712 0.5712 0.5712 0.5712 0.5712 0.5712 | 1.1567 1.2008 1.1854 1.1726 1.1717 1.0850 | 96.8 102.0 100.9 99.0 96.5 95.8 | 98.5 | 2.59 |
Embodiment 9
The preparation of blank liquid takes by weighing other flavour of a drug by recipe quantity with mensuration except that Fructus Aurantii, make the preparation that does not contain Fructus Aurantii by formulation and technology, make blank liquid by the need testing solution preparation method, measurement result is seen Fig. 1, Fig. 2 and Fig. 3 illustrate that other medicinal materials and auxiliary material all do not disturb the mensuration of aurantiin.
Embodiment 10
Sample determination is got ten batches of stomach and intestine peace samples, is equipped with need testing solution by need testing solution preparation below legal system, two parts of need testing solutions of every batch of preparation.Accurate need testing solution, each 2 μ l of reference substance solution of drawing inject high performance liquid chromatograph, measure, and ten batch samples the results are shown in Table 2.
The measurement result of aurantiin in table 2 gastrointestinal disease treating pill
Table2 Determination of Naringin in Weichang’an Pill
| Lot number | Naringin content (mg/g) |
| D109004 | 4.8 |
| D109007 | 4.9 |
| D109008 | 5.2 |
| D109009 | 5.4 |
| D109010 | 4.6 |
| D109016 | 5.6 |
| D109019 | 5.3 |
| D109020 | 4.4 |
| 030681 | 4.6 |
| 030784 | 4.8 |
| Mean value | 4.98 |
By naringin content in ten batches of gastrointestinal disease treating pills being detected, obtaining mean value is 4.98mg/g, and the standard that the suggestion gastrointestinal disease treating pill increases measuring naringin content is decided to be: naringin content must not be less than 4.38mg/g in the gastrointestinal disease treating pill.
This assay method easily and fast, specificity and favorable reproducibility, the result can be used for the quality control of gastrointestinal disease treating pill accurately and reliably.
Discuss
Extracting method is investigated: bibliographical information, aurantiin is soluble in organic solvent, and extracting method mainly contains ultrasonic and refluxing extraction, compares by adopting methyl alcohol ultrasonic Extraction and methanol eddy to extract, the result is best with the methanol eddy extraction effect, so adopt this extracting method.
The selection of moving phase: successively test methanol-water, acetonitrile-water, methyl alcohol-0.3 glacial acetic acid, acetonitrile-0.3% glacial acetic acid etc. and be moving phase, experimentize, compare the HPLC spectrogram, it is that moving phase detects that the result shows with acetonitrile-0.3% glacial acetic acid (20: 80), the sample peak separates best, so preferred acetonitrile-0.3% glacial acetic acid (20: 80) is a moving phase.
Claims (8)
1. the assay method of naringin content in the gastrointestinal disease treating pill is characterized in that being made up of following steps:
(1) it is an amount of that the aurantiin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 0.0119mg/ml～0.119mg/ml, in contrast product solution;
(2) the gastrointestinal disease treating pill porphyrize is got in the preparation of need testing solution, it is fixed to get the accurate title of powder 0.1g, put 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, water-bath reflux 20～90 minutes, put and be chilled to room temperature, the accurate title, decide, and supplies with methyl alcohol to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and 0.1%～1% glacial acetic acid aqueous solution is 10～50: 90～50, and the concentration of described glacial acetic acid aqueous solution is concentration of volume percent; Detect wavelength: 217nm; Flow velocity: 0.5ml/min～1.0ml/min; 20 ℃～40 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
2. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1, the concentration that it is characterized in that described reference substance solution is 0.01mg/ml.
3. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1 is characterized in that the described water-bath reflux time is 30 minutes.
4. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1 is characterized in that described miillpore filter aperture is 0.45 μ m.
5. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1, the concentration that it is characterized in that described glacial acetic acid aqueous solution is 0.3%.
6. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1, the volume ratio that it is characterized in that described acetonitrile and glacial acetic acid is 20: 80, the concentration of described glacial acetic acid aqueous solution is 0.3%.
7. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1 is characterized in that described flow velocity is 0.8ml/min.
8. the assay method of naringin content in a kind of gastrointestinal disease treating pill according to claim 1 is characterized in that described column temperature is 35 ℃.
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| CN101757293B (en) * | 2008-12-24 | 2012-02-29 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Quality control method of gastrointestinal disease treating pill |
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| CN1487279A (en) * | 2003-05-29 | 2004-04-07 | 江西江中药业股份有限公司 | Quality detection method for compound pummelo exocarp prepn |
| CN1528773A (en) * | 2003-09-29 | 2004-09-15 | 中山大学 | Method for extracting shaddock ped aglycone from shaddock |
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| CN101757293B (en) * | 2008-12-24 | 2012-02-29 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Quality control method of gastrointestinal disease treating pill |
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Address after: 300380 Yumen Road, Xiqing District, Tianjin Patentee after: Lerentang Pharmaceutical Factory of Jinyao Darentang Group Co.,Ltd. Address before: 300380 Yumen Road, Xiqing District, Tianjin Patentee before: Letrentang pharmaceutical factory of Tianjin Zhongxin Pharmaceutical Group Co.,Ltd. |
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