CN1831518A - Quick monitoring method for elution start or end of column separation eluent of Chinese medicine - Google Patents
Quick monitoring method for elution start or end of column separation eluent of Chinese medicine Download PDFInfo
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Abstract
A method for quickly detecting out elution initial point or end point of eluant in column separation for Chinese traditional medicine is finalized mainly by measuring refractivity as sampling eluant to be detected continuously as per interval in 0.01 - 20 times volume of each column eluant then measuring refractivity of eluant sample.
Description
Technical field
The present invention relates to the column separation eluent elution start of Chinese medicine or the method for supervising of terminal point.Particularly the column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point.Method for rapidly monitoring is mainly finished by the index of refraction measurement.The another kind of expression way of the present invention is: index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point.
To declare especially in addition be post separate with column chromatography be equal notion, different experts have two kinds of calls to its appellation in academia, but express equivalent in meaning, post of the present invention separates and all is meant the technology of separating heterogeneity with post with column chromatography.
Background technology
Column separation process is the process that a kind of different molecular is separated from each other, when a biased sample is imported in the support of a stationary phase, and another fluid is a mobile phase when passing through, because each component of sample and stationary phase and mobile phase is interactional varies in size make each component must separate by the speed difference of stationary phase support.
Post separates according to the separation principle difference and is divided into the separation of distribution post, adsorption column separation, ion exchange column separation, the separation of exclusion post etc.According to the difference of biased sample component type, the separatory stationary phase of post is also different, and stationary phase commonly used has macroreticular resin, silica gel, polyamide, aluminium oxide, zeyssatite etc.
At present, it is more and more that post is separated in Chinese medicine scientific research, production application, but still lack standard, maturation, complete, technology efficiently so far in application.Especially operate for judgement or " the blind method " of column separation eluent starting point and terminal point, most of operators judge eluent starting point and terminal point according to the situation of movement of chromatographic band in the change color of eluent and the pillar, are difficult to ensure stable, the homogeneous of product quality.
" blind method " judgement is subjected to the influence of subjective factor many, and is inconsistent with the target that the modernization of Chinese medicine needs monitoring quick and precisely to produce.
Can accurately monitor production by the detection of UV method, the detection of HPLC method, but the shortcoming that the UV method detects, the HPLC method detects is time-consuming, can not finish the target that quick monitoring is produced.The UV method of each Chinese medicine system detects, the HPLC method detects all needs according to different Chinese medicine system configurations related solution, adjusts measurement parameter.Even fixed production and UV method, HPLC method detecting operation rules, the data of UV method, HPLC method were reported minimum need consuming time tens to tens of minutes, the time of this consumption in operation and manpower are enough to offset its accurately advantage of monitoring production, allow the experience decision operation of " blind method " return real production control on the contrary.
In the Chinese medicine of reality is produced, because of Chinese medicine material from different places, the time of purchase is also different, batch difference that causes Chinese medicine material, so when relying on the middle pharmaceutically active ingredient that post separates or the column chromatography technology acquisition is different, even at same Chinese medicine, the starting point of eluent or terminal point are all variant each time.Influence because of batch difference of Chinese medicine material, it is accurate inadequately relying on fixing production operation to come the separating traditional Chinese medicine composition, best mode is to monitor the starting point or the terminal point of eluent simply, accurately and rapidly, thereby adjust the kind of the consumption and the replacing eluent of eluent immediately, be beneficial to modernization of Chinese medicine production.
And " blind method " and the UV method, the HPLC method that rely on subjective experience to judge at present all can't solve the starting point of monitoring eluent simply, fast or the technical requirement of terminal point simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of column separation eluent elution start of the starting point of eluent or the method for terminal point, particularly Chinese medicine or method for rapidly monitoring of terminal point monitored simply, fast.
Purpose of the present invention also can be: index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point.
Technical scheme of the present invention is:
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by the 0.01-20 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by the 0.1-2 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by the 0.2-1 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: database is set up or do not set up to the index of refraction data that will measure the eluent sample, and data are carried out or do not handled.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: described Chinese medicine is any class in single medicinal material material, kinds of traditional Chinese medicines material, single medicinal material preparation, compound Chinese medicinal preparation, the Chinese and Western medicine compound preparation.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: the used stationary phase of post separation of Chinese medicine can be any one in resin, silica gel, gel, polyamide, aluminium oxide, the zeyssatite, and wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it is macroreticular resin that the post of Chinese medicine separates used stationary phase resin.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: eluent can be water, the single or organic solvent that mixes.
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point.
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point, wherein: by the 0.1-2 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point, wherein: by the 0.2-1 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Method for rapidly monitoring is mainly finished by the index of refraction measurement.
The principle of the invention is that shown index of refraction is different when containing heterogeneity according to different solutions, and the proportional relation of the concentration of solution and index of refraction adopts the starting point and the terminal point of index determination method coupled columns separating traditional Chinese medicine composition wash-out to detect judgement within the specific limits.In order to achieve the above object, the present invention has studied sample on different Chinese crude drugs and the compound preparation sample, wash-out, the process of detection.
The present invention adopt the refractive power instrument--handheld refractometer, Abbe refractometer etc. is a kind of instrument of measuring constituent concentration in the solution by refractive index.All solution all can make direction of light generation deviation.The deviation of light can increase with the increase of solution composition concentration.Its operating process is that sample drop 2-3 is dripped to the refractometer minute surface, regulates eyepiece, makes dark side clear, and the scale value of dark boundary line correspondence is by being surveyed the refractive power value.
The invention has the advantages that:
Refractometry of the present invention has the starting point of monitoring eluent simply, fast or the advantage of terminal point.Refractometry detects with respect to detection methods such as HPLC, UV commonly used more easy, and operability is stronger.This method can be implemented in line and detects in real time, and experimental result is more stable accurately, and needed instrument and equipment is simple simultaneously, operates also very convenient easy row, is applicable to laboratory study and commercial production, uses very extensive.
The effective constituent Changing Pattern is similar substantially in the eluent of refractometry and UV method, HPLC method.But the mode difference of three's method projection, refractometry is shown the influence of whole composition to refractive power; The UV method is shown the influence of certain constituents to uv absorption; The HPLC method is only shown the Changing Pattern of single composition; Refractometry the back both easy, quick, low cost and other advantages are arranged, shortcoming be sensitivity not as good as the back both.But refractometry is quicker than UV method, HPLC method in monitoring industrial processes, and good practicability is arranged.The needs that adapt to the actual production monitoring.
Because the present invention emphasizes practicality, emphasize to adapt to fast the actual production monitoring, the requirement of accuracy is lowerd a little, under common situation, directly by the variation of index of refraction, understand and starting point or the terminal point of monitoring eluent just can play than the better effect of blind method.Under common situation, do not need as UV method at a slow speed, the degree of accuracy the HPLC method.
But in order better to guarantee the degree of accuracy of monitoring fast, can carry out data processing,, can judge the starting point or the terminal point of monitoring eluent more intuitively so that after the variation amplification with index of refraction to the variation of index of refraction.
In the part test example, for example test example 4,5, index of refraction is not carried out data processing, also can help to judge the starting point or the terminal point of eluent.But index of refraction is carried out data processing, for example test example 1,2,3, can monitor the starting point or the terminal point of eluent more accurately.If the index of refraction of testing example 1,2,3 is not carried out data processing certainly, equally also can judge the starting point or the terminal point of monitoring eluent.
Description of drawings: Figure of description 1-18 by test test the collection of illustrative plates of data.Detailed content is seen each test example.
Specific embodiment
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.01 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.05 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.1 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.15 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.2 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 0.8 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 1 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 1.5 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 2 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 3 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Embodiment 11
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 5 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 8 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Embodiment 13
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 10 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 15 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: by 20 times interval of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: 5 points are got at 2.0 times interval by every post effluent volume continuously, get 5 points continuously by 1.0 times interval of every post effluent volume again, get 10 points continuously by 0.3 times interval of every post effluent volume again, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Embodiment 17
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: 3 points are got at 4.0 times interval by every post effluent volume continuously, get 10 points continuously by 1.0 times interval of every post effluent volume again, get 20 points continuously by 0.1 times interval of every post effluent volume again, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: database is set up or do not set up to the index of refraction data that will measure the eluent sample, and data are carried out or do not handled.
Embodiment 19
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: described Chinese medicine is the single medicinal material material, repeats above-mentioned all embodiment respectively.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: described Chinese medicine is the kinds of traditional Chinese medicines material, repeats above-mentioned all embodiment respectively.
Embodiment 21
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: described Chinese medicine is compound Chinese medicinal preparation, repeats above-mentioned all embodiment respectively.
Embodiment 22
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: described Chinese medicine is the Chinese and Western medicine compound preparation, repeats above-mentioned all embodiment respectively.
Embodiment 23
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be resin that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
Embodiment 24
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be silica gel that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be gel that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
Embodiment 26
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be polyamide that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
Embodiment 27
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be aluminium oxide that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
Embodiment 28
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it can be zeyssatite that the post of Chinese medicine separates used stationary phase, wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.Repeat above-mentioned all embodiment respectively.
Embodiment 29
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: it is macroreticular resin that the post of Chinese medicine separates used stationary phase resin.Repeat above-mentioned all embodiment respectively.
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: eluent can be a water.Repeat above-mentioned all embodiment respectively.
Embodiment 31
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: eluent can be single organic solvent.Repeat above-mentioned all embodiment respectively.
Embodiment 32
The column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point, wherein: eluent can be the organic solvent that mixes.Repeat above-mentioned all embodiment respectively.
Embodiment 33
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point.
Embodiment 34
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point, wherein: by the 0.1-2 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point, wherein: by the 0.2-1 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
Attached part test example in addition:
Following instantaneously changing eluent or finally stop using certain eluent all to rely on the timing monitoring index of refraction to make a decision in the test example.
Test example 1
Chinese crude drug or compound preparation obtain Chinese crude drug extract and compound preparation extract through handling, and sample on the extract is put in the chromatographic column of having handled well, the moving phase wash-out, and eluent detects.
Macroporous absorbent resin (Macfofeticulaf Resin) is a class organic polymer adsorbent that grows up sixties end, has porous network structure and absorption property preferably, can be by physisorption adsorb organic compound selectively from aqueous solution.Its suction-operated is to finish by surface adsorption, surface electrical behavior or formation hydrogen bond.Macroporous absorbent resin has been widely used in fields such as wastewater treatment, medical industry, clinical identification and food at present.And the macroporous resin adsorption isolation technics is just progressively to be applied to Chinese herbal medicine effective ingredients the end of the seventies in last century to extract a kind of separating and purifying technology that separates, it mainly is to adopt special adsorbent, selectively adsorbs effective constituent wherein, a kind of extraction refining process of removal invalid components from the Chinese medicine compound prescription decocting liquid.This technology can make effective component highly enriched, and impurity reduces, and also can reduce the moisture absorption of product, effectively removes heavy metal, solves the difficult problem of Chinese medicine heavy metals exceeding standard.
The column chromatographic isolation and purification technological process of salviamiltiorrhizabung is schematically as follows:
The red rooted salvia extract is crossed the AB-8 macroreticular resin and is detected
1, the extraction of red rooted salvia: get red rooted salvia 200g, add 10 times of amounts of distilled water, extract 2 times, each 1 hour, merge extract, centrifugal, behind the concentrating under reduced pressure (70 ℃), adding distil water makes and is dissolved to 500ml.
2, go up sample wash-out and detection: get extract 50ml, last sample (2cm * 80cm resin column, AB-8 resin 40ml), dynamically after the absorption, distilled water wash-out, then 80% ethanol elution behind 30% ethanol elution, 10ml/ part is collected, and with handing the index of refraction that saccharimeter (WYT-32 type) detects critical drop, per 0.5 bed volume detects uv absorption, and pure wash-out partly merges per 1 bed volume HPLC method and detects tanshin polyphenolic acid B, relatively three's testing result.
Wherein the numerical value of elution volume is meant the multiple of every post bed volume.In following table, be meant 0.25 times interval, get eluent sample to be detected continuously, measure the index of refraction of eluent sample by every post bed volume effluent volume.
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water |
| Elution volume | 0 | 0.25 | 0.50 | 0.75 | 1.00 | 1.25 | 1.50 | 1.75 | 2.00 | 2.25 | 2.50 |
| The index of refraction value | 15.5 | 15.8 | 15.8 | 9.6 | 5.0 | 2.6 | 1.4 | 0.8 | 0.6 | 0.2 | 0.1 |
| Value of magnification | 25.7 | 25.8 | 25.8 | 23.3 | 20.1 | 16.8 | 13.7 | 10.9 | 9.5 | 4.0 | 0.5 |
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol |
| Elution volume | 2.75 | 3.00 | 3.25 | 3.50 | 3.75 | 4.00 | 4.25 | 4.50 | 4.75 | 5.00 | 5.25 |
| The index of refraction value | 0 | 0 | 0 | 0 | 0 | 0 | 0.2 | 4.0 | 9.8 | 11.4 | 11.2 |
| Value of magnification | 0 | 0 | 0 | 0 | 0 | 0 | 4.0 | 19.0 | 23.4 | 11.5 | 10.2 |
| The wash-out solvent | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol | 30% ethanol |
| Elution volume | 5.50 | 5.75 | 6.00 | 6.25 | 6.50 | 6.75 | 7.00 | 7.25 | 7.50 | 7.75 | 8.00 |
| The index of refraction value | 11.0 | 11.0 | 10.8 | 10.6 | 10.6 | 10.6 | 10.6 | 10.5 | 10.5 | 10.5 | 10.5 |
| Value of magnification | 8.5 | 8.5 | 6.0 | 0.5 | 0.5 | 0.5 | 0.5 | 0 | 0 | 0 | 0 |
| The wash-out solvent | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol | 80% ethanol |
| Elution volume | 8.25 | 8.50 | 8.75 | 9.00 | 9.25 | 9.50 | 9.75 | 10.00 | 10.25 | 10.50 | 10.75 |
| The index of refraction value | 10.5 | 10.6 | 10.8 | 11.4 | 17.2 | 19.2 | 19.5 | 19.6 | 19.6 | 19.5 | 19.5 |
| Value of magnification | 0 | 0.5 | 6 | 11.5 | 21.5 | 22.8 | 23.0 | 0.5 | 0.5 | 0 | 0 |
The red rooted salvia extract is crossed AB-8 macroreticular resin eluent ultraviolet method testing result
| The wash-out solvent | Distilled water | |||||||
| Elution volume (bed volume) | 0 | 0.50 | 1.00 | 1.50 | 2.00 | 2.50 | 3.00 | 3.50 |
| Ultraviolet absorption value | 1.851 | 1.365 | 0.976 | 0.581 | 0.352 | 0.114 | 0.057 | 0.021 |
| The wash-out solvent | 30% ethanol | |||||||
| Elution volume (bed volume) | 4.00 | 4.50 | 5.00 | 5.50 | 6.00 | 6.50 | 7.00 | 7.50 |
| Ultraviolet absorption value | 0.018 | 0.359 | 0.855 | 1.675 | 1.056 | 0.585 | 0.210 | 0.095 |
| The wash-out solvent | 80% ethanol | ||||||
| Elution volume (bed volume) | 8.00 | 8.50 | 9.00 | 9.50 | 10.00 | 10.50 | 10.75 |
| Ultraviolet absorption value | 0.161 | 0.417 | 1.021 | 0.787 | 0.442 | 0.291 | 0.120 |
The red rooted salvia extract is crossed AB-8 macroreticular resin eluent HPLC and is detected the tanshin polyphenolic acid B result
| 30% | 30% ethanol elution amount |
| 1BV | 69.15mg |
| 2BV | 182.23 mg |
| 3BV | 48.94mg |
| 4BV | 33.84mg |
| 5BV | 8.34mg |
| 6BV | 0mg |
Wherein: resin volume 40ml, applied sample amount 466mg, effluent content 13mg, water elution liquid hold-up 47.5mg, adsorbance 405,5mg, desorption amount 342.5mg, desorption rate 84.46%.
Interpretation of result: the result by refractometry and UV method and HPLC method judgement eluent initial point and terminal point has consistance, and the result is that water elution 3.5BV is the initial point of 30% ethanol elution, and 30% ethanol elution is complete to 7BV effective constituent wash-out, and reach home this moment.Three result relatively, refractometry is obviously easy, quick than UV method, HPLC method, easy operating, and refractometry is at the globality of traditional Chinese medicine ingredients, UV, HPLC method are at local or single.
Test example 2: red spoon medicinal material is crossed the AB-8 resin
One: application process
1.1, sample preparation:
Take by weighing red spoon medicinal material 200g, 8 times of medicinal material amount distilled water refluxing extraction twice, 1h/ time, merge extract, concentrating sample liquid is to 4 times of medicinal material amounts, and it is 60% that the adding absolute ethyl alcohol transfers to concentration of alcohol, leave standstill back overnight and filter, recovered under reduced pressure is not to there being the alcohol flavor, and adding distil water makes into 800ml.Accurate two parts of the 200ml that draw dynamically go up AB-8 macroporous absorbent resin (wet resin 40ml is equivalent to 28g) respectively, the ethanol elution of water-40%, and every 10ml collects, the online detection of refractometry, a HPLC method detects Paeoniflorin, and a UV method detects Paeoniflorin.
1.2, determining alcohol detects:
The accurate 5ml that draws puts in the 25ml volumetric flask in the eluent that 10ml collects, and adds distilled water to scale, and the alcoholic degree meter detects concentration of alcohol.
| Concentration of | 5 | 10 | 15 | 20 | 25 | 30 | 35 | 40 |
| The refractive power value | 1.9 | 3.4 | 5.3 | 6.6 | 8.7 | 9.8 | 11.6 | 13.2 |
Ethanol refractive power linear relationship chart is seen Figure of description 1
Two: detect data:
2.1, refractometry detects number
Detect the refractive power data No. 1
| Elution volume (BV) | Index of refraction | Value of magnification | Determining alcohol (%) | |
| | 0 | 6.4 | 21.28 | |
| Distilled water | 0.25 | 6 | 20.96 | |
| Distilled water | 0.50 | 6 | 20.96 | |
| Distilled water | 0.75 | 5 | 20.05 | |
| Distilled water | 1.00 | 3 | 17.49 | |
| Distilled water | 1.25 | 1.5 | 14.03 | |
| Distilled water | 1.50 | 1 | 12.00 | |
| Distilled water | 1.75 | 0.9 | 11.47 | |
| Distilled water | 2.00 | 0.6 | 9.45 | |
| Distilled water | 2.25 | 0.6 | 9.45 | |
| Distilled water | 2.50 | 0.4 | 7.42 | |
| Distilled water | 2.75 | 0.4 | 7.42 | |
| Distilled water | 3.00 | 0.4 | 7.42 | |
| Distilled water | 3.25 | 0.3 | 5.98 | |
| Distilled water | 3.50 | 0 | 0.00 | |
| Distilled water | 3.75 | 0 | 0.00 | |
| 40% ethanol | 4.00 | 0 | 0.00 | |
| 40% ethanol | 4.25 | 3 | 17.49 | 5％ |
| 40% ethanol | 4.50 | 13 | 24.82 | 11％ |
| 40% ethanol | 4.75 | 16.5 | 18.26 | 28％ |
| 40% ethanol | 5.00 | 16 | 17.49 | 34％ |
| 40% ethanol | 5.25 | 15 | 15.47 | 40％ |
| 40% ethanol | 5.50 | 14.4 | 13.68 | |
| 40% ethanol | 5.75 | 13.8 | 10.88 | |
| 40% ethanol | 6.00 | 13.5 | 8.53 | |
| 40% ethanol | 6.25 | 13.4 | 7.42 |
| 40% ethanol | 6.50 | 13.3 | 5.98 | |
| 40% ethanol | 6.75 | 13.2 | 3.95 | |
| 40% ethanol | 7.00 | 13.1 | 0.49 | |
| 40% ethanol | 7.25 | 13 | 0.00 | |
| 40% ethanol | 7.50 | 13 | 0.00 | |
| 40% ethanol | 7.75 | 13 | 0.00 | |
| 40% ethanol | 8.00 | 13 | 0.00 |
No. 1 eluent alcohol graded detects data
| Elution volume (BV) | Eluent refractive power value | Concentration of alcohol (%) | Ethanol refractive power value | Composition refractive power value behind the deduction ethanol |
| 4.25 | 3.0 | 5％ | 1.9 | 1.1 |
| 4.50 | 13.0 | 11％ | 3.8 | 9.2 |
| 4.75 | 16.5 | 28％ | 9.3 | 7.2 |
| 5.00 | 16.0 | 34％ | 11.3 | 4.7 |
| 5.25 | 15.0 | 40％ | 13.0 | 2 |
Detect the refractive power data No. 2
| Elution volume (BV) | Index of refraction | Value of | |
| 0 | 6.6 | 21.44 | |
| Distilled water | 0.25 | 6.7 | 21.51 |
| Distilled water | 0.50 | 6.6 | 21.44 |
| Distilled water | 0.75 | 5 | 20.05 |
| Distilled water | 1.00 | 2.8 | 17.15 |
| Distilled water | 1.25 | 1.5 | 14.03 |
| Distilled water | 1.50 | 1 | 12.00 |
| Distilled water | 1.75 | 0.8 | 10.88 |
| Distilled water | 2.00 | 0.7 | 10.22 |
| Distilled water | 2.25 | 0.6 | 9.45 |
| Distilled water | 2.50 | 0.6 | 9.45 |
| Distilled water | 2.75 | 0.4 | 7.42 |
| Distilled water | 3.00 | 0.4 | 7.42 |
| Distilled water | 3.25 | 0.3 | 5.98 |
| Distilled water | 3.50 | 0 | 0.00 |
| Distilled water | 3.75 | 0 | 0.00 |
| Distilled water | 4.00 | 0 | 0.00 |
| 40% ethanol | 4.25 | 0.7 | 10.22 |
| 40% ethanol | 4.50 | 12.8 | 24.75 |
| 40% ethanol | 4.75 | 17.2 | 19.18 |
| 40% ethanol | 5.00 | 16.2 | 17.82 |
| 40% ethanol | 5.25 | 15.4 | 16.38 |
| 40% ethanol | 5.50 | 14.4 | 13.68 |
| 40% ethanol | 5.75 | 14 | 12.00 |
| 40% ethanol | 6.00 | 13.7 | 10.22 |
| 40% ethanol | 6.25 | 13.4 | 7.42 |
| 40% ethanol | 6.50 | 13.3 | 5.98 |
| 40% ethanol | 6.75 | 13.2 | 3.95 |
| 40% ethanol | 7.00 | 13.1 | 0.49 |
| 40% ethanol | 7.25 | 13 | 0.00 |
| 40% ethanol | 7.50 | 13 | 0.00 |
| 40% ethanol | 7.75 | 13 | 0.00 |
| 40% ethanol | 8.00 | 13 | 0.00 |
No. 2 eluent alcohol graded detects data
| Elution volume (BV) | Eluent refractive power value | Concentration of alcohol (%) | Ethanol refractive power value | Composition refractive power value behind the deduction ethanol |
| 4.25 | 0.7 | Be lower than detectability | - | - |
| 4.50 | 12.8 | 10％ | 3.3 | 9.5 |
| 4.75 | 17.2 | 30％ | 7.3 | 9.9 |
| 5.00 | 16.2 | 35％ | 10.3 | 5.9 |
| 5.25 | 15.4 | 40％ | 13.0 | 2.4 |
Detect the refractive power variation diagram No. 1 and see Figure of description 2
Deduction ethanol background refractive power variation diagram is seen Figure of description 3
Detect the refractive power variation diagram No. 2 and see Figure of description 4
2.2, the UV method detects data
Testing conditions: wavelength 230nm
Detection method: (concentration: 0.0192mg/ml) be contrast, detect absorption under 230nm, the absorption value of No. 2 samples is calculated paeoniflorin content with one point external standard method with Paeoniflorin.The absorption value of Paeoniflorin is 1.514Abs.
No. 2 UV detects the Paeoniflorin data
| The wash-out solvent | Elution volume | Ultraviolet absorption value | Extension rate | Paeoniflorin content (mg) |
| - | 0 | 3.067 | 5000 | 1944.73 |
| Distilled water | 0.25 | 1.053 | 1000 | 133.54 |
| Distilled water | 0.75 | 0.965 | 1000 | 122.38 |
| Distilled water | 1.25 | 0.747 | 1000 | 94.73 |
| Distilled water | 1.75 | 0.761 | 500 | 48.25 |
| Distilled water | 2.25 | 0.882 | 100 | 11.19 |
| Distilled water | 2.75 | 0.766 | 50 | 4.86 |
| Distilled water | 3.25 | 0.662 | 50 | 4.20 |
| Distilled water | 3.75 | 0.616 | 50 | 3.91 |
| 40% ethanol | 4.25 | 2.331 | 1000 | 295.61 |
| 40% ethanol | 4.75 | 3.510 | 1000 | 445.13 |
| 40% ethanol | 5.25 | 3.714 | 1000 | 471.00 |
| 40% ethanol | 5.75 | 1.615 | 500 | 102.40 |
| 40% ethanol | 6.25 | 0.995 | 100 | 12.62 |
| 40% ethanol | 6.75 | 0.764 | 50 | 4.84 |
| 40% ethanol | 7.25 | 0.653 | 50 | 4.14 |
| 40% ethanol | 7.75 | 0.600 | 50 | 3.80 |
| 40 | 8 | 0.581 | 50 | 3.68 |
| - | Effluent | 0.115 | 100/250 | 36.46 |
No. 2 UV detect the paeoniflorin content changing trend diagram and see Figure of description 5
2.3, the HPLC method detects the Paeoniflorin data
Testing conditions: enlightening horse C
18Post (post number 8032165), methanol-water-glacial acetic acid (34.5-65-0.5), wavelength: 2230nm, flow velocity 1.0ml/min
Detection method:
The accurate sample liquid 4ml that draws adds water to 50ml, detects as extract.
No. 1 40% ethanol eluate is mixed by 1 bed volume, add 40% ethanol and be settled to 50ml, filtering membrane detects.
Paeoniflorin concentration 0.03mg/ml, peak area: 216.5 (5ul)
HPLC method inspection paeoniflorin content data
| Elution volume (BV) | Sample size | Peak area | Content (mg) | Adsorbance (mg) | Desorption rate (%) |
| 4 | 0.2 | 0 | 0.00 | 1080.01 | 75.52 |
| 5 | 0.2ul | 3243.3 | 531.92 | ||
| 6 | 0.2ul | 1478.3 | 242.45 | ||
| 7 | 0.2ul | 251.7 | 41.28 | ||
| 8 | 0.2 | 0 | 0.00 | ||
| Chinese herbaceous peony water extract | 5.0ul | 5554.6 | |||
| Water lotion | 0.2ul | 665.3 | |||
| Effluent | 0.2ul | 239.5 |
Red spoon is crossed AB-8 resin HPLC detection paeoniflorin content variation diagram and is seen Figure of description 6
Test example 3 roots of kudzu vine, Radix Glycyrrhizae, Jingzhi Guanxin tablet prescription be the part collection of illustrative plates as a result
One, the root of kudzu vine is crossed AB-8 resin testing result
Root of kudzu vine medicinal material is crossed AB-8 resin elution liquid refractive power detected value and is seen Figure of description 7.
Root of kudzu vine medicinal material is crossed AB-8 resin elution liquid UV detection flavonoid content figure (249nm) and is seen Figure of description 8.
The AB-8 resin elution liquid HPLC method of crossing root of kudzu vine medicinal material detects puerarin content figure and sees Figure of description 9.
Radix Glycyrrhizae crosses D-101 resin testing result
Licorice medicinal materials is crossed D-101 resin elution liquid refractive power detected value and is seen Figure of description 10.
Licorice medicinal materials is crossed D-101 resin elution liquid UV detection figure (500nm) and is seen Figure of description 11.
Licorice medicinal materials is crossed D-101 resin elution liquid HPLC detection glycyrrhizic acid content figure and is seen Figure of description 12.
Jingzhi Guanxin tablet (compound dalbergia wood) is crossed the D-101 resin
Jingzhi Guanxin tablet (compound dalbergia wood) is crossed D-101 resin elution liquid refractometry testing result and is seen Figure of description 13.
Jingzhi Guanxin tablet (compound dalbergia wood) is crossed D-101 resin elution liquid UV testing result (wavelength 276nm calculates 276nm with tanshinone IIA and absorbs the contained content of material of eluent just) and is seen Figure of description 14.
Jingzhi Guanxin tablet (compound dalbergia wood) is crossed D-101 resin elution liquid HPLC method detection content of danshinolic acid B and be the results are shown in Figure of description 15.
Test example 4
The application of the present invention in the compound preparation column separating purification: Jingzhi Guanxin tablet prescription extract is crossed the D-101 resin and is detected
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water |
| Elution volume | 0.25 | 0.50 | 0.75 | 1.00 | 1.25 | 1.50 | 1.75 | 2.00 | 2.25 | 2.50 | 2.75 |
| The index of refraction value | 9.9 | 9.8 | 5.2 | 1.8 | 1.0 | 0.8 | 0.4 | 0.3 | 0.3 | 0.3 | 0.3 |
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water |
| Elution volume | 3.00 | 3.25 | 3.50 | 3.75 | 4.00 | 4.25 | 4.50 | 4.75 | 5.00 | 5.25 | 5.50 |
| The index of refraction value | 0.2 | 0.2 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0.5 |
| The wash-out solvent | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol |
| Elution volume | 5.75 | 6.00 | 6.25 | 6.50 | 6.75 | 7.00 | 7.25 | 7.50 | 7.75 | 8.00 | 8.25 |
| The index of refraction value | 1.1 | 1.3 | 1.4 | 1.9 | 2.7 | 3.5 | 4.2 | 4.5 | 6.4 | 8.9 | 9.3 |
| The wash-out solvent | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | |
| Elution volume | 8.50 | 8.75 | 9.00 | 9.25 | 9.50 | 9.75 | 10.00 | 10.25 | 10.50 | ||
| The index of refraction value | 9.3 | 8.6 | 8.1 | 7.5 | 7.0 | 6.3 | 6.2 | 5.2 | 4.6 | ||
| The wash-out solvent | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | 20% ethanol | ||
| Elution volume | 10.75 | 11.00 | 11.25 | 11.50 | 11.75 | 12.00 | 12.25 | 12.50 | 12.75 | ||
| The index of refraction value | 3.8 | 3.5 | 3.5 | 3.5 | 3.5 | 3.5 | 3.7 | 4.8 | 6.9 | ||
| The wash-out solvent | 20% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | ||
| Elution volume | 13.00 | 13.25 | 13.50 | 13.75 | 14.00 | 14.25 | 14.50 | 14.75 | 15.00 | ||
| Refractive power | 7.0 | 7.0 | 7.9 | 8.6 | 12.0 | 14.3 | 15.0 | 15.7 | 15.6 |
| The rate value | |||||||||||
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | ||
| Elution volume | 15.25 | 15.50 | 15.75 | 16.00 | 16.25 | 16.50 | 16.75 | 17.00 | 17.25 | ||
| The index of refraction value | 15.6 | 15.3 | 15 | 14.1 | 12.0 | 9.9 | 8.6 | 8.6 | 8.0 | ||
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | ||
| Elution volume | 17.50 | 17.75 | 18.00 | 18.25 | 18.50 | 18.75 | 19.00 | 19.25 | 19.50 | ||
| The index of refraction value | 7 | 6.1 | 5.8 | 5.6 | 5.6 | 5.5 | 5.5 | 5.5 | 5.5 | ||
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | ||||||
| Elution volume | 19.75 | 20.25 | 20.50 | 20.75 | 21.00 | ||||||
| The index of refraction value | 5.5 | 5.5 | 5.5 | 5.5 | 5.5 |
The HPLC method is measured paeoniflorin content and be the results are shown in Figure of description 16
| Peak area | Content (mg) | ||
| Water lotion | 271 | 16.04943 | |
| Effluent | 172.7 | 10.22781 | |
| Extract | 581.2 | 172.102 | |
| 6 | 21~24 | 197.4 | 2.338124 |
| 7 | 25~28 | 479 | 5.673563 |
| 8 | 29~32 | 365.4 | 4.328016 |
| 9 | 33~36 | 290.8 | 3.444409 |
| 10 | 37~40 | 213.6 | 2.530006 |
| 11 | 41~44 | 161.5 | 1.912903 |
| 12 | 45~48 | 654.6 | 7.753474 |
| 13 | 49~52 | 966.1 | 28.60767 |
| 14 | 53~56 | 806.7 | 23.88759 |
| 15 | 57~60 | 722.1 | 21.38246 |
| 16.5 | 63~66 | 312.4 | 9.250632 |
| 20 | 67~80 | 300.4 | 8.895294 |
| 21 | 81~84 | 47 | 1.39174 |
| The desorption rate | 633.2 | 83.25％ |
The HPLC method detects the paeoniflorin content trend map and sees Figure of description 17
Test example 5
The application of the present invention in the compound preparation column separating purification: smart safflower extract is crossed the HPD-700 resin and is detected
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water |
| Elution volume | 0.25 | 0.50 | 0.75 | 1.00 | 1.25 | 1.50 | 1.75 | 2.00 | 2.25 | 2.50 | 2.7 5 |
| The index of refraction value | 17 | 16.8 | 15.2 | 11.8 | 8.0 | 6.8 | 6.4 | 5.3 | 4.7 | 4.3 | 3.3 |
| The wash-out solvent | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water | Distilled water |
| Elution volume | 3.00 | 3.25 | 3.50 | 3.75 | 4.00 | 4.25 | 4.50 | 4.75 | 5.00 | 5.25 | 5.5 0 |
| The index of refraction value | 2.9 | 2.2 | 1.5 | 1 | 0.6 | 0.3 | 0.2 | 0 | 0 | 0 | 0 |
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | |
| Elution volume | 5.75 | 6.00 | 6.25 | 6.50 | 6.75 | 7.00 | 7.25 | 7.50 | 7.75 | 8.00 | |
| The index of refraction value | 0 | 0.3 | 1.4 | 2.9 | 4.7 | 7.5 | 9.2 | 10.5 | 11.4 | 11.9 | |
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | |
| Elution volume | 8.25 | 8.50 | 8.75 | 9.00 | 9.25 | 9.50 | 9.75 | 10.00 | 10.25 | 10.50 | |
| The index of refraction value | 11.9 | 12.0 | 12.1 | 12.3 | 12.5 | 13.0 | 13.3 | 15.2 | 16.2 | 17.6 | |
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | |
| Elution volume | 10.75 | 11.00 | 11.25 | 11.50 | 11.75 | 12.00 | 12.25 | 12.50 | 12.75 | 13.00 | |
| The index of refraction value | 17.0 | 16.5 | 15.8 | 15.5 | 15.5 | 15.5 | 14.9 | 14.8 | 14.9 | 15.0 | |
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | |
| Elution volume | 13.25 | 13.50 | 13.75 | 14.00 | 14.25 | 14.50 | 14.75 | 15.00 | 15.25 | ||
| The index of refraction value | 14.0 | 13.9 | 12.6 | 10.0 | 9.3 | 8.1 | 7.7 | 6.4 | 5.6 | ||
| The wash-out solvent | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | 50% ethanol | ||||
| Elution volume | 15.50 | 15.75 | 16.00 | 16.25 | 16.50 | 16.75 | 17.00 | ||||
| The index of refraction value | 5.3 | 5.3 | 5.3 | 5.3 | 5.3 | 5.3 | 5.3 |
The HPLC method is measured carthamus tinctorius yellow color content and be the results are shown in following table and Figure of description 18
| Content (mg) | |
| Water lotion | 130.05 |
| Effluent | 120.23 |
| Extract | 1172.11 |
| 6 | 20.34 |
| 7 | 50.11 |
| 8 | 113.16 |
| 9 | 130.68 |
| 10 | 207.54 |
| 11 | 181.92 |
| 12 | 127.79 |
| 13 | 109.57 |
| 14 | 78.89 |
| 15 | 41.38 |
In above-mentioned test example 5, the wash-out terminal point of distilled water eluent is that 5.75 times of every post effluent volume are located; Simultaneously 5.75 times of every post effluent volume to locate also be the elution start of 50% ethanolic solution; It is the wash-out terminal point of 50% ethanolic solution that 17.00 times of every post effluent volume are located.
In above-mentioned test example 1, the wash-out terminal point of distilled water eluent is that 4.00 times of every post effluent volume are located; Simultaneously 4.00 times of every post effluent volume to locate also be the elution start of 30% ethanolic solution; The wash-out terminal point of distilled water eluent is that 8.25 times of every post effluent volume are located; Simultaneously 8.25 times of every post effluent volume to locate also be the elution start of 80% ethanolic solution; It is the wash-out terminal point of 80% ethanolic solution that 10.75 times of every post effluent volume are located.
The elution start in other test examples or the division of wash-out terminal point are similarly.
In above-mentioned test example 1, if before 8.25 times of every post effluent volume are located, just change 80% ethanol in advance, the part composition that meaning should be dissolved in 30% ethanolic solution may be sneaked in the next step, both lost the composition in the previous step, made again that the material purity in the next step was not enough.And if after 8.25 times of every post effluent volume are located, just change 80% ethanol, meaning has been wasted 30% ethanolic solution.
If can judge immediately that monitoring elution start or wash-out terminal point obviously can reduce above-mentioned separation situation impure or the waste eluent and take place.
Claims (10)
1, the column separation eluent elution start of Chinese medicine or the method for rapidly monitoring of terminal point is characterized in that: by the 0.01-20 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
2, the column separation eluent elution start of Chinese medicine as claimed in claim 1 or the method for rapidly monitoring of terminal point, it is characterized in that: by the 0.1-2 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
3, the column separation eluent elution start of Chinese medicine as claimed in claim 1 or the method for rapidly monitoring of terminal point, it is characterized in that: by the 0.2-1 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
4, as claim 1 or the column separation eluent elution start of 2 or 3 described Chinese medicines or the method for rapidly monitoring of terminal point, it is characterized in that: database is set up or do not set up to the index of refraction data that will measure the eluent sample, and data are carried out or do not handled.
5, as claim 1 or the column separation eluent elution start of 2 or 3 described Chinese medicines or the method for rapidly monitoring of terminal point, it is characterized in that: described Chinese medicine is any class in single medicinal material material, kinds of traditional Chinese medicines material, single medicinal material preparation, compound Chinese medicinal preparation, the Chinese and Western medicine compound preparation.
6, as claim 1 or the column separation eluent elution start of 2 or 3 described Chinese medicines or the method for rapidly monitoring of terminal point, it is characterized in that: the used stationary phase of post separation of Chinese medicine can be any one in resin, silica gel, gel, polyamide, aluminium oxide, the zeyssatite, and wherein detecting the used instrument and equipment of eluent is the instrument and equipment that utilizes the refraction principle design.
7, the column separation eluent elution start of Chinese medicine as claimed in claim 6 or the method for rapidly monitoring of terminal point is characterized in that: it is macroreticular resin that the post of Chinese medicine separates used stationary phase resin.
8, as claim 1 or the column separation eluent elution start of 2 or 3 described Chinese medicines or the method for rapidly monitoring of terminal point, it is characterized in that: eluent can be water, the single or organic solvent that mixes.
9, index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point.
10, index of refraction is measured the application in the quick monitoring of the column separation eluent elution start of Chinese medicine or terminal point, it is characterized in that: by the 0.01-20 interval doubly of every post effluent volume, get eluent sample to be detected continuously, measure the index of refraction of eluent sample.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101984343A (en) * | 2010-10-22 | 2011-03-09 | 浙江大学 | Method of discriminating key points in macroporous resin separation and purification process of traditional Chinese medicines |
| CN105223162A (en) * | 2015-09-29 | 2016-01-06 | 山东万邦赛诺康生化制药股份有限公司 | A kind of production liquaemin process wash-out method for supervising |
| CN105842195B (en) * | 2016-03-24 | 2018-12-14 | 安徽华润金蟾药业股份有限公司 | The judgment method of cream terminal is received in cinobufagin concentration |
| CN110567915A (en) * | 2019-09-06 | 2019-12-13 | 云南大唐汉方制药股份有限公司 | online detection method for ethanol concentration in dragon blood residue steaming process |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6377341B1 (en) * | 1999-08-03 | 2002-04-23 | University Technology Corporation | Refractive index based detector system for liquid chromatography |
| US6816248B2 (en) * | 2001-04-26 | 2004-11-09 | Reichert, Inc. | Hand-held automatic refractometer |
| CN1403809A (en) * | 2001-09-04 | 2003-03-19 | 洪筱坤 | Establishment and application of Chinese medicine chaacteristic fingerprint spectrum |
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2005
- 2005-12-19 CN CNB2005101205103A patent/CN100445730C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101984343A (en) * | 2010-10-22 | 2011-03-09 | 浙江大学 | Method of discriminating key points in macroporous resin separation and purification process of traditional Chinese medicines |
| CN105223162A (en) * | 2015-09-29 | 2016-01-06 | 山东万邦赛诺康生化制药股份有限公司 | A kind of production liquaemin process wash-out method for supervising |
| CN105223162B (en) * | 2015-09-29 | 2018-03-30 | 山东万邦赛诺康生化制药股份有限公司 | One kind production liquaemin process elution monitoring method |
| CN105842195B (en) * | 2016-03-24 | 2018-12-14 | 安徽华润金蟾药业股份有限公司 | The judgment method of cream terminal is received in cinobufagin concentration |
| CN110567915A (en) * | 2019-09-06 | 2019-12-13 | 云南大唐汉方制药股份有限公司 | online detection method for ethanol concentration in dragon blood residue steaming process |
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