CN100401057C - Method for detecting aloes glucoside in compounded aloes capsule - Google Patents
Method for detecting aloes glucoside in compounded aloes capsule Download PDFInfo
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- CN100401057C CN100401057C CNB2005101112594A CN200510111259A CN100401057C CN 100401057 C CN100401057 C CN 100401057C CN B2005101112594 A CNB2005101112594 A CN B2005101112594A CN 200510111259 A CN200510111259 A CN 200510111259A CN 100401057 C CN100401057 C CN 100401057C
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Abstract
The invention supplies a testing method to test the barbaloin in compound aloe capsule that has strong specificity. And it could effectively control the quality of compound aloe capsule.
Description
Technical field:
The present invention relates to technical field of traditional Chinese medicines.Be specifically related to barbaloin content detecting method in a kind of compound aloe capsule.
Background technology:
Compound aloe capsule record in＜＜People's Republic of China's drug standards promulgated by the ministries or commissions of the Central Government the 18 in Chinese traditional patent formulation preparation, prescription is made up of aloe, amber, cinnabar, indigo naturalis, aloe is a monarch drug in a prescription in the prescription, but the content assaying method of no barbaloin in its quality standard.In order to control product quality better, formulated this detection method.
Cardinal rule according to content of drug mensuration, the assay project should be the monarch drug in a prescription in the prescription, valuable medicine, and aloe is monarch drug in a prescription in prescription, so select to detect the aloe in the prescription, the principal ingredient of aloe is a barbaloin, so with the detection index of the barbaloin detection index as compound aloe capsule.
Summary of the invention:
Technical matters to be solved by this invention is to design a kind of to carrying out the method for barbaloin content separation detection in the compound aloe capsule, thereby controls product quality effectively.
The invention provides barbaloin content detecting method in a kind of compound aloe capsule.
The object of the invention can be realized by following proposal:
One, instrument, reagent and confession test agent
Instrument: UV-200II type high performance liquid chromatograph, UV-200II type ultraviolet variable-wavelenght detector, Echrom98 chromatographic data work of treatment station
Reagent: barbaloin standard items, acetonitrile, methyl alcohol are chromatographically pure level reagent, and other reagent is analyzes pure level reagent.
Supply test agent: compound aloe capsule
Chromatographic condition
Chromatographic column: Hyper 0DS2C18,4.6 * 250mm
Moving phase: acetonitrile-0.1% trifluoracetic acid-tetrahydrofuran (150-250: 750-850: 2-5)
Flow velocity: 1ml/min
Detect wavelength: 355nm
Column temperature: room temperature.
Two, test method and result
(1) preparation of reference substance solution:
Precision takes by weighing barbaloin reference substance 12.5mg, puts in the 25ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up; Precision is measured 5ml, puts in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up, promptly;
(2) preparation of need testing solution
Get the content of 10 of compound aloe capsules, mix; Get 0.2 gram, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 20ml that adds, close plug claims to decide weight, and sonicated 30min is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, discard filtrate just, precision is measured subsequent filtrate 5ml, put in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shake up, filter with miillpore filter (0.45um), get subsequent filtrate, promptly;
(3) assay method
Accurate respectively reference substance and each 20u1 sample introduction of need testing solution drawn injects high performance liquid chromatograph, measures, and calculates, promptly.
Three, the technical standard of Jian Ceing
Every (0.5g) compound aloe capsule contains barbaloin 〉=7.5mg
Four, the feasibility of this detection method can be described by following test
1. the preparation of negative control solution
According to the prescription of compound aloe capsule, the analog sample that the technology preparation lacks aloe, make the compound aloe capsule negative control solution according to the need testing solution preparation method.
2. the investigation of linear relationship
Precision takes by weighing the barbaloin reference substance, adds the solution that methyl alcohol is mixed with 0.5mg/m1, and it is an amount of to get this solution, is diluted to 0.01,0.02,0.05,0.1,0.2 with methyl alcohol, the solution of 0.3mg/ml.Get above-mentioned solution 20ul sample introduction, measure according to the chromatographic condition worked out, record peak area and sample size are horizontal ordinate with the reference substance concentration of sample introduction, are ordinate with the peak area, the drawing standard curve.Regression equation is Y=365195X-1322.3 R=0.9993, becomes good linear relationship between the range of linearity 0.2-10ug. linear relationship is investigated and be the results are shown in Table 1, the typical curve See Figure
Table 1 barbaloin linear relationship is investigated the result
| Barbaloin reference substance concentration (mg/ml) | 0.01 | 0.02 | 0.05 | 0.1 | 0.2 | 0.3 | 0.5 |
| The peak area of measuring | 3459.52 | 7355.75 | 17771.60 | 34841.38 | 69714.04 | 104008.94 | 184522.95 |
Get same reference substance solution and need testing solution, respectively 0,2, sample introduction was measured in 4,6,20,24 hours.RSD to the product peak area is 0.33% (n=6), and the RSD of test sample peak area is 0.29% (n=6), illustrates that barbaloin is stable in 24 hours at least, and stability test the results are shown in Table 2
Table 2 stability test result
| Time (hour) | Barbaloin reference substance peak area | The test sample peak area |
| 0 | 17052.32 | 12123.97 |
| 2 | 17079.19 | 12083.13 |
| 4 | 17078.44 | 12039.67 |
| 6 | 17142.32 | 12014.69 |
| 20 | 17027.42 | 12037.61 |
| 24 | 17166.04 | 12069.81 |
| Mean value | 17090.955 | 12061.48 |
| RSD | 0.33％ | 0.29％ |
3. precision test
Accurate reference substance solution and each 20ul of need testing solution (lot number 050611) of drawing repeats sample introduction 5 times, measures peak area, and the result shows, the RSD=0.43% of reference substance peak area (n=5); Test sample peak area RSD=0.81% (n=5). the result shows that degree of accuracy is good.The degree of accuracy test findings sees Table 3.
Table 3 Precision test result
| Mensuration number of times numbering | Barbaloin reference substance peak area | The test sample peak area |
| 1 | 16918.8 | 12193.25 |
| 2 | 17076.83 | 12019.77 |
| 3 | 17052.32 | 12218.29 |
| 4 | 17109.36 | 12068.04 |
| 5 | 17077.25 | 12011.01 |
| Mean value | 17046.912 | 12102.072 |
| RSD | 0.43％ | 0.81％ |
4. replica test
Get compound aloe capsule (lot number 050611) and carry out parallel assay 5 times, calculate content, recording every, to contain barbaloin mean value be 17.602mg, and RSD=0.26% (n=5) illustrates this assay method good reproducibility.Replica test the results are shown in Table 4
Table 4 compound aloe capsule replica test result
| Numbering | Barbaloin content (mg/ grain) |
| 1 | 17.54 |
| 2 | 17.57 |
| 3 | 17.65 |
| 4 | 17.63 |
| 5 | 17.62 |
| Mean value | 17.602 |
| RSD | 0.26％ |
5. specificity test
Under the chromatographic condition of drafting, accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects high performance liquid chromatograph respectively, measures.The result shows that the test sample degree of separation is better, and retention time is moderate, and barbaloin is consistent in the retention time of reference substance and peak and the test sample.
The accurate negative control product solution 20ul that draws injects high performance liquid chromatograph, measures.The result shows, in the negative control chromatogram, with the relevant position at barbaloin reference substance peak on, noiseless peak occurs, and illustrates that the medicinal material of other except that aloe does not have influence to measurement result in the compound aloe capsule, promptly negative control is noiseless.
6. average recovery test
Take the test of application of sample absorption method.Get the compound aloe capsule (lot number 050613 of known content, content 21.13mg/ grain) 10 intragranulars are tolerant, mix, get above-mentioned medicinal powder 0.2g, the accurate title, decide, 5 parts of nominals, and each adds a certain amount of barbaloin reference substance respectively, make the application of sample need testing solution according to the need testing solution preparation method, measure.Test findings shows that five times average recovery rate is 100.33%, and RSD=0.44% illustrates that this assay method measurement result is accurate.The average recovery test findings sees Table 5
Table 5 barbaloin application of sample reclaims experimental result
This assay method specificity is strong, and the linearity of method, stability, reappearance, average recovery all reach technical requirement preferably.The inventive method can effectively be controlled the product quality of compound aloe capsule.
Embodiment
One, instrument, reagent and confession test agent
Instrument: UV-200II type high performance liquid chromatograph, UV-200II type ultraviolet variable-wavelenght detector, Echrom98 chromatographic data work of treatment station
Reagent: barbaloin standard items, acetonitrile, methyl alcohol are chromatographically pure level reagent, and other reagent is analyzes pure level reagent.
Supply test agent: the compound aloe capsule sample
Chromatographic condition
Chromatographic column: Hyper 0DS2C18,4.6 * 250mm
Moving phase: acetonitrile-0.1% trifluoracetic acid-tetrahydrofuran (180: 820: 2.5)
Flow velocity: 1ml/min
Detect wavelength: 355nm
Column temperature: room temperature.
Two, test method and result
1. the preparation of reference substance solution:
Precision takes by weighing barbaloin reference substance 12.5mg, puts in the 25ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up; Precision is measured 5ml, puts in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up, promptly.
2. the preparation of need testing solution
Get the content of 10 of compound aloe capsules, mix; Get 0.2 gram, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 20ml that adds, close plug claims to decide weight, and sonicated 30min is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, discard filtrate just, precision is measured subsequent filtrate 5ml, put in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shake up, filter with miillpore filter (0.45um), get subsequent filtrate, promptly.
3. assay method
Respectively accurate reference substance and each 20ul sample introduction of need testing solution drawn injects high performance liquid chromatograph, measures, and calculates, and gets promptly that to contain barbaloin content be 8.5mg.
Claims (1)
1. barbaloin content detecting method in the compound aloe capsule: it is characterized in that this method comprises the following steps:
(1) preparation of reference substance solution: precision takes by weighing barbaloin reference substance 12.5mg, puts in the 25ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up; Precision is measured 5ml, puts in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shakes up, promptly;
(2) preparation of need testing solution: get the content of 10 of compound aloe capsules, mix; Get 0.2 gram, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 20ml that adds, close plug claims to decide weight, and sonicated 30min is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, discard filtrate just, precision is measured subsequent filtrate 5ml, put in the 50ml volumetric flask, with dissolve with methanol and be diluted to scale, shake up, filter with miillpore filter 0.45um, get subsequent filtrate, promptly;
(3) chromatographic condition of high performance liquid chromatograph: chromatographic column: Hyper 0DS2C18,4.6 * 250mm; Moving phase: acetonitrile-0.1% trifluoracetic acid-tetrahydrofuran 150-250: 750-850: 2-5; Flow velocity: 1ml/min; Detect wavelength: 355nm; Column temperature: room temperature;
(4) assay method: accurate respectively reference substance and each 20ul sample introduction of need testing solution drawn, inject high performance liquid chromatograph, measure, calculate, promptly get every 0.5g compound aloe capsule and contain barbaloin 〉=7.5mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101112594A CN100401057C (en) | 2005-12-08 | 2005-12-08 | Method for detecting aloes glucoside in compounded aloes capsule |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101112594A CN100401057C (en) | 2005-12-08 | 2005-12-08 | Method for detecting aloes glucoside in compounded aloes capsule |
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| Publication Number | Publication Date |
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| CN1979156A CN1979156A (en) | 2007-06-13 |
| CN100401057C true CN100401057C (en) | 2008-07-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005101112594A Active CN100401057C (en) | 2005-12-08 | 2005-12-08 | Method for detecting aloes glucoside in compounded aloes capsule |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104181238A (en) * | 2013-05-22 | 2014-12-03 | 河北万邦复临药业有限公司 | Barbaloin detection method |
| CN114965748A (en) * | 2022-04-28 | 2022-08-30 | 陕西科技大学 | Method for simultaneously detecting barbaloin, aloe-emodin and indirubin in new compound aloe capsule |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174023A (en) * | 1997-01-30 | 1998-02-25 | 北京轻工业学院海口技工贸实业开发公司 | Aloe cosmetics series prepared with aloe as main material |
| WO2005112962A1 (en) * | 2004-05-21 | 2005-12-01 | Shunichi Yagi | Aloe powder, aloe juice, and method for producing the same |
-
2005
- 2005-12-08 CN CNB2005101112594A patent/CN100401057C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174023A (en) * | 1997-01-30 | 1998-02-25 | 北京轻工业学院海口技工贸实业开发公司 | Aloe cosmetics series prepared with aloe as main material |
| WO2005112962A1 (en) * | 2004-05-21 | 2005-12-01 | Shunichi Yagi | Aloe powder, aloe juice, and method for producing the same |
Non-Patent Citations (4)
| Title |
|---|
| RP-HPLC法测定芦荟中芦荟苷的含量. 张永文等.中草药，第30卷第8期. 1999 |
| RP-HPLC法测定芦荟中芦荟苷的含量. 张永文等.中草药，第30卷第8期. 1999 * |
| 木立芦荟中芦荟苷的HPLC分析及抗氧化性能测定. 侯冬岩等.分析测试学报，第24卷第1期. 2005 |
| 木立芦荟中芦荟苷的HPLC分析及抗氧化性能测定. 侯冬岩等.分析测试学报，第24卷第1期. 2005 * |
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Owner name: HEBEI WANBANGFULIN MEDICINE INDUSTRY CO., LTD. Free format text: FORMER NAME: SHANGHAI FUXING LINXI MEDICINE INDUSTRY CO., LTD. |
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Address after: 88, Ping An street, Linxi County, Hebei Province, zip code: 054900 Co-patentee after: Shanghai Fuxing Pharmaceutical (Group) Co., Ltd. Patentee after: Hebei Wanbang Adventist Pharmaceutical Co. Ltd. Address before: 88, Ping An street, Linxi County, Hebei Province, zip code: 054900 Co-patentee before: Shanghai Fuxing Pharmaceutical (Group) Co., Ltd. Patentee before: Shanghai Fuxing Linxi Pharmaceutical Co., Ltd. |