CN107894473A - A kind of HPLC methods of rhizome of Chinese monkshood acid content in detection tuber of pinellia - Google Patents
A kind of HPLC methods of rhizome of Chinese monkshood acid content in detection tuber of pinellia Download PDFInfo
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Abstract
The invention provides purposes of the method for rhizome of Chinese monkshood acid content in the detection tuber of pinellia in tuber of pinellia quality testing, the invention provides a kind of HPLC methods for detecting rhizome of Chinese monkshood acid content in the tuber of pinellia in addition.The inventive method can accurately and efficiently detect cis, trans-aconitic acid content in the tuber of pinellia, to improve the quality control level of the tuber of pinellia, promoting the utilization of medicinal material to lay a good foundation.
Description
Technical field
The present invention relates to a kind of HPLC methods for detecting rhizome of Chinese monkshood acid content in the tuber of pinellia.
Background technology
The tuber of pinellia is Araeceae Pinellia the tuber of pinellia Pinellia ternata (Thunb.) Breit dry tuber.
With eliminating dampness and eliminating phlegm, stopping nausea and vomiting by lowering the adverse flow of QI, the effect of dissolving lump and resolving mass.Trembled with fear phlegm for damp phlegm, cough and phlegm, phlegm retention anti-dazzle nervous, anemophlegmatic vertigo,
Phlegm and headache, vomiting gastric disorder causing nausea, chest gastral cavity ruffian, globus hysteriocus；Controlling outward carbuncle swells subcutaneous nodule.
Tuber of pinellia complicated component, containing a variety of organic acids, alkaloid, albumen etc., wherein organic acid is that it plays curative effect
A kind of important effective component.The current often evaluation criteria using succinic acid content as tuber of pinellia quality, such as Chinese Pharmacopoeia 2015
Potentiometric titration is used in version, measure total organic acids content is calculated with succinic acid content, quality control is carried out to the tuber of pinellia.This method
Complex operation, it is vulnerable to the influence of other organic acids and operating condition, error is larger, and metering is not accurate enough, to the quality of the tuber of pinellia
Control unsatisfactory.Also there is containing for the organic acids such as a small amount of document report measure tuber of pinellia mesoxalic acid, malic acid, citric acid, butanedioic acid
Amount, but evaluation index is still not perfect enough.
Therefore, in order to the tuber of pinellia overall quality control, it is necessary to further find the tuber of pinellia in organic acidity test evaluation index
And assay method.
The content of the invention
It is an object of the invention to provide a kind of new method that quality testing is carried out to the tuber of pinellia.
Inventor has found that the tuber of pinellia contains 2 kinds of cis-aconitic, trans-aconitic acid new organic acids first under study for action, and
Separation and assay have been carried out to it.
The invention provides purposes of the method for rhizome of Chinese monkshood acid content in the detection tuber of pinellia in tuber of pinellia quality testing.
Wherein, the aconitic acid is cis and/or trans-aconitic acid.
The invention provides a kind of method for detecting rhizome of Chinese monkshood acid content in the tuber of pinellia, step are as follows：
A, need testing solution is prepared：
Pinellia Tuber is taken, ultrasonic extraction, centrifugation, takes supernatant, the acid that phosphorates mixes, and is extracted with ethyl acetate, is evaporated, with stream
Dynamic phased soln, obtains need testing solution；
B, reference substance solution is prepared：
Cis-aconitic and/or trans-aconitic acid reference substance are taken, water dissolving, obtains reference substance solution；
C, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
Chromatographic column：C18 chromatographic columns；
Mobile phase：Mobile phase is the phosphoric acid solution (3~10 of methanol (or acetonitrile) -0.1%:97~90)；
Detection wavelength：210nm；
D, cis-aconitic and/or trans-aconitic acid content in the tuber of pinellia are calculated according to testing result.
Wherein, in step a, the Extraction solvent of ultrasonic extraction is water or 80% methanol.
Wherein, per 1g Pinellia Tubers, the dosage of water is 20~50mL；Preferably, per 1g Pinellia Tubers 50mL water.
Wherein, in step a, per 25ml supernatants 0.1ml phosphoric acid；And/or the extraction times of ethyl acetate are 5 times.
Wherein, the time of the ultrasonic extraction is 15~120 minutes；Preferably, the time of extraction is 60 minutes.
Wherein, in step c, the specification of the chromatographic column is：Internal diameter 4.6mm, length 250mm, 5 μm of packing material size；It is preferred that
Chromatographic column model Inertsil ODS-3C18 chromatographic columns.
Wherein, in step c, mobile phase is the phosphoric acid solution of methanol -0.1% (3:97), the phosphoric acid solution of acetonitrile -0.1% (3:
Or the phosphoric acid solution of methanol -0.1% (10 97):90).
Wherein, the column temperature of the chromatographic condition is 25~35 DEG C；Flow velocity is 0.5~0.8mL/min；
Preferably, column temperature is 35 DEG C；Flow velocity is 0.8mL/min.
Inventor has been successfully established cis, trans crow in the measure tuber of pinellia by the screening to extracting method and chromatographic condition
The HPLC methods of head acid content, this method accurately and reliably, it is easy quick, be the organic acid content analysis of the tuber of pinellia, improve the tuber of pinellia
Overall quality control is laid a good foundation, and is advantageous to the utilization of Pinellia Ternate, is had a good application prospect.
Obviously, according to the above of the present invention, according to the ordinary technical knowledge and customary means of this area, do not departing from
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The embodiment of form by the following examples, the above of the present invention is remake further specifically
It is bright.But the scope that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following example.It is all to be based on the above of the present invention
The technology realized belongs to the scope of the present invention.
Brief description of the drawings
Fig. 1 blank sample HPLC chromatograms.
Fig. 2 reference substance HPLC collection of illustrative plates figures；Wherein, 1 is cis-aconitic, and 2 be trans-aconitic acid.
Fig. 3 pinellia sample HPLC collection of illustrative plates (method of embodiment 1)；Wherein, 1 is cis-aconitic, and 2 be trans-aconitic acid.
Fig. 4 pinellia sample HPLC collection of illustrative plates (method of embodiment 2)；Wherein, 1 is cis-aconitic, and 2 be trans-aconitic acid.
Fig. 5 pinellia sample HPLC collection of illustrative plates (method of embodiment 3)；Wherein, 1 is cis-aconitic, and 2 be trans-aconitic acid.
Fig. 6 pinellia sample HPLC collection of illustrative plates (method of embodiment 4)；Wherein, 1 is cis-aconitic, and 2 be trans-aconitic acid.
Embodiment
It is described further below with embodiment, but the present invention is not limited to these embodiments.
The HPLC methods of the present invention of embodiment 1
Method is as follows：
1st, need testing solution is prepared：
Pinellia sample powder (cross No. four sieve) about 1g is taken, it is accurately weighed, put in 150ml conical flasks, add water 50mL, it is weighed heavy
Amount, it is ultrasonically treated 60 minutes, lets cool, then weighed weight, the weight of less loss to be supplied with water, is centrifuged, precision measures supernatant 25mL,
Phosphorate sour 0.1mL, shakes up, and is extracted with ethyl acetate 5 times, each 20mL, combined ethyl acetate, is evaporated, and residue adds methanol (or second
Nitrile) -0.1% phosphoric acid solution (3:97) dissolve, and be settled to 5mL, filter, take subsequent filtrate, produce.
2nd, reference substance solution is prepared
Precision weighs reference substance cis-aconitic, trans-aconitic acid, water dissolving, shakes up, produces.
Prepare blank sample：The preparation method of blank sample is as follows：150ml conical flasks are taken, add water 50mL, weighed weight,
It is ultrasonically treated 60 minutes, lets cool, then weighed weight, the weight of less loss is supplied with water, is centrifuged, precision measures clarified solution 25mL, added
Phosphoric acid 0.1mL, shakes up, and is extracted with ethyl acetate 5 times, each 20mL, combined ethyl acetate, is evaporated, residue adds methanol -0.1%
Phosphoric acid solution (3:97) dissolve, and be settled to 5mL, filter, take subsequent filtrate, produce.
3rd, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
The high performance liquid chromatograph of Agilent 1200 (DAD detectors), Inertsil ODS-3C18 (4.6 × 250mm, 5 μm)
Chromatographic column, with the phosphoric acid solution of methanol -0.1% (3:97) it is mobile phase；Flow velocity：0.8mL/min, Detection wavelength 210nm；Column temperature
For 35 DEG C.
4th, cis-aconitic in the tuber of pinellia, trans-aconitic acid content are calculated according to testing result.
Measurement result is shown in Fig. 1-3.
It can be seen that the inventive method can effectively determine cis-aconitic and trans-aconitic acid in the tuber of pinellia.
The HPLC methods of the present invention of embodiment 2
Method is as follows：
1st, need testing solution is prepared：With embodiment 1.
2nd, reference substance solution is prepared：With embodiment 1.
3rd, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
The high performance liquid chromatograph of Agilent 1200 (DAD detectors), Inertsil ODS-3C18 (4.6 × 250mm, 5 μm)
Chromatographic column, with the phosphoric acid solution of acetonitrile -0.1% (3:97) it is mobile phase；Flow velocity：0.8mL/min, Detection wavelength 210nm；Column temperature
For 35 DEG C.
4th, cis-aconitic in the tuber of pinellia, trans-aconitic acid content are calculated according to testing result.
Measurement result is shown in Fig. 4.
It can be seen that the inventive method can effectively determine cis-aconitic and trans-aconitic acid in the tuber of pinellia.
The HPLC methods of the present invention of embodiment 3
Method is as follows：
1st, need testing solution is prepared：With embodiment 1.
2nd, reference substance solution is prepared：With embodiment 1.
3rd, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
The high performance liquid chromatograph of Agilent 1200 (DAD detectors), Inertsil ODS-3C18 (4.6 × 250mm, 5 μm)
Chromatographic column, with the phosphoric acid solution of methanol -0.1% (3:97) it is mobile phase；Flow velocity：0.5mL/min, Detection wavelength 210nm；Column temperature
For 25 DEG C.
4th, cis-aconitic in the tuber of pinellia, trans-aconitic acid content are calculated according to testing result.
Measurement result is shown in Fig. 5.
It can be seen that the inventive method can effectively determine cis-aconitic and trans-aconitic acid in the tuber of pinellia.
The HPLC methods of the present invention of embodiment 4
Method is as follows：
1st, need testing solution is prepared：With embodiment 1.
2nd, reference substance solution is prepared：With embodiment 1.
3rd, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
The high performance liquid chromatograph of Agilent 1200 (DAD detectors), Inertsil ODS-3C18 (4.6 × 250mm, 5 μm)
Chromatographic column, with the phosphoric acid solution of methanol -0.1% (10:90) it is mobile phase；Flow velocity：0.5mL/min, Detection wavelength 210nm；Post
Temperature is 25 DEG C.
4th, cis-aconitic in the tuber of pinellia, trans-aconitic acid content are calculated according to testing result.
Measurement result is shown in Fig. 6.
It can be seen that the inventive method can effectively determine cis-aconitic and trans-aconitic acid in the tuber of pinellia.
Beneficial effects of the present invention are illustrated below by way of test example：
The technological parameter screening of the inventive method of test example 1
First, experiment material
1st, crude drug source
Pinellia Ternate, Nanchong City Pengan County of Sichuan Province tuber of pinellia experimental plot is picked up from, removed the peel, drying forms.
2nd, instrument, reagent, reagent
The high performance liquid chromatograph of Agilent 1200 (DAD detectors)；Inertsil ODS-3C18 (4.6 × 250mm, 5 μm)
Chromatographic column, electronic balance (Sai Duolisi scientific instrument Co., Ltd)；Water-bath (Beijing Zhong Xing great achievements Instrument Ltd.)；It is dry
Dry case；Rotary Evaporators (German Heldolph)；Multiplex vavuum pump of circulating water type；The speed governing of HY-4A digital displays uses oscillator；Centrifugation
Machine (U.S. Beckmancoulter).
It is micro- big that cis-aconitic, trans-aconitic acid are purchased from middle section, purity ＞ 98%.
Methanol, acetonitrile, ethyl acetate, phosphoric acid are chromatographically pure, and water is ultra-pure water, and other are pure to analyze.
2nd, the screening of the inventive method
(1) preparation of reference substance solution
Precision weighs reference substance cis-aconitic, trans-aconitic acid 10.20mg, 11.46mg respectively, water dissolving, shakes up, i.e.,
.
(2) preparation of need testing solution
Inventor is investigated to the extracting method of test sample, Extraction solvent, extraction time and post processing extraction solvent consumption, tool
Body is as follows：
1st, the investigation of extracting method
Pinellia sample powder (crossing No. four sieves) 1g is taken, it is accurately weighed, add water 50mL, weighed weight, be ultrasonically treated or heat
Backflow 60 minutes, is let cool, then weighed weight, and the weight of less loss, centrifugation are supplied with water, and precision measures supernatant 25mL, and phosphorate acid
0.1mL, shake up, be extracted with ethyl acetate 5 times, each 20mL, combined ethyl acetate, be evaporated, residue add methanol (or acetonitrile)-
0.1% phosphoric acid solution (3:97) dissolve, and be settled to 5mL, filter, take subsequent filtrate, produce.
The μ l of need testing solution 20 are taken, inject high performance liquid chromatograph, it is molten with the mixing of cis-aconitic and trans-aconitic acid
Liquid is reference substance, calculates the content of 2 kinds of aconitic acids.
Chromatographic condition is as follows：With Inertsil ODS-3C18 (4.6 × 250mm, 5 μm) for chromatographic column, with methanol -0.1%
Phosphoric acid solution (3:97) it is mobile phase；Flow velocity：0.8mL/min, Detection wavelength 210nm；Column temperature is 35 DEG C.
It the results are shown in Table 1.
The different extracting mode results of table 1
As shown in Table 1, only ultrasonic extracting method can extract 2 kinds of aconitic acids, and reflux extraction method can not extract to obtain 2
Kind of aconitic acid, and in extraction process, heating and refluxing extraction high temperature is easily caused the starch gelatinization in the tuber of pinellia, be unfavorable for it is follow-up from
The extraction of the heart and composition.
Therefore, selection ultrasonic extracting method prepares testing sample.
2nd, the investigation of Extraction solvent
From different solvents, other methods according to above-mentioned ultrasonic extraction, investigate water and 80% methanol, two kinds of extractions are molten
The influence of agent.It the results are shown in Table 2.
The different solvents result of table 2
As shown in Table 2,2 kinds of solvents can extract aconitic acid, wherein, the extraction effect of water is best.Therefore, water is selected
For Extraction solvent.
2nd, the investigation of extraction time
By the method for above-mentioned ultrasonic extraction, using water as Extraction solvent, supersound process 15,30,60,120min, extraction is investigated
Time.It the results are shown in Table 3.
The different extraction time results of table 3
As shown in Table 3,2 kinds of aconitic acids can be effectively extracted when ultrasonic time is 30-120min, it is not same in order to ensure
The abundant extraction of product, extraction time selection 60min.
4th, the investigation of post processing extraction solvent consumption
Sample powder (crossing No. four sieves) about 1g is taken, it is accurately weighed, add water 20mL, 30mL, 40,50mL, weighed weight, ultrasound
60min is handled, is let cool, then weighed weight, the weight of less loss to be supplied with water, is centrifuged, precision measures supernatant, and phosphorate sour 0.1mL,
Shake up, be extracted with ethyl acetate 5 times, each 20mL, combined ethyl acetate, be evaporated, residue adds the phosphorus of methanol (or acetonitrile) -0.1%
Acid solution (3:97) dissolve, and be settled to 5mL, filter, take subsequent filtrate, produce.Investigate extraction time.
The μ l of need testing solution 20 are taken, inject high performance liquid chromatograph, it is molten with the mixing of cis-aconitic and trans-aconitic acid
Liquid is reference substance, calculates the content of 2 kinds of aconitic acids.
Chromatographic condition is as follows：With Inertsil ODS-3C18 (4.6 × 250mm, 5 μm) for chromatographic column, with methanol -0.1%
Phosphoric acid solution (3:97) it is mobile phase；Flow velocity：0.8mL/min, Detection wavelength 210nm；Column temperature is 35 DEG C.It the results are shown in Table 4.
The different solvents dosage of table 4 investigates result
As shown in Table 4,2 kinds of aconitic acids can be effectively extracted when water consumption is 20-50ml, due to tuber of pinellia content of starch compared with
Height, Pinellia Tuber is not easy to disperse when liquid volume is less, therefore preferably 50ml is advisable.
Therefore, the optimal need testing solution preparation method finally determined is：Sample powder (crossing No. four sieves) 1g is taken, it is accurate
It is weighed, put in conical flask with cover, add water 50mL, weighed weight, be ultrasonically treated 60 minutes, let cool, then weighed weight, supplied with water
The weight of less loss, centrifugation, precision measures supernatant 25mL, and phosphorate sour 0.1mL, shakes up, and is extracted with ethyl acetate 5 times, every time
20mL, combined ethyl acetate, it is evaporated, residue adds the phosphoric acid solution (3 of methanol (or acetonitrile) -0.1%:97) dissolve, and be settled to
5mL, filtration, takes subsequent filtrate, produces.
To sum up, the present inventor has found under study for action, and the tuber of pinellia contains 2 kinds of cis-aconitic, trans-aconitic acid new organic acids,
And by the screening to extracting method and chromatographic condition, it has been successfully established cis, trans-aconitic acid content in the measure tuber of pinellia
HPLC methods, this method accurately and reliably, it is easy quick, be the organic acid content analysis of the tuber of pinellia, improve the total quality control of the tuber of pinellia
System is laid a good foundation, and is advantageous to the utilization of Pinellia Ternate, is had a good application prospect.
Claims (10)
1. detect purposes of the method for rhizome of Chinese monkshood acid content in the tuber of pinellia in tuber of pinellia quality testing.
2. purposes according to claim 1, it is characterised in that：The aconitic acid is cis and/or trans-aconitic acid.
A kind of 3. method for detecting rhizome of Chinese monkshood acid content in the tuber of pinellia, it is characterised in that：Step is as follows：
A, need testing solution is prepared：
Pinellia Tuber is taken, ultrasonic extraction, centrifugation, takes supernatant, the acid that phosphorates mixes, and is extracted with ethyl acetate, is evaporated, uses mobile phase
Dissolving, obtains need testing solution；
B, reference substance solution is prepared：
Cis-aconitic and/or trans-aconitic acid reference substance are taken, water dissolving, obtains reference substance solution；
C, it is respectively that need testing solution and reference substance solution injection high performance liquid chromatograph detection, chromatographic condition is as follows：
Chromatographic column：C18 chromatographic columns；
Mobile phase：Mobile phase is the phosphoric acid solution (3~10 of methanol (or acetonitrile) -0.1%:97~90)；
Detection wavelength：210nm；
D, cis-aconitic and/or trans-aconitic acid content in the tuber of pinellia are calculated according to testing result.
4. HPLC methods according to claim 3, it is characterised in that：In step a, the Extraction solvent of ultrasonic extraction for water or
80% methanol.
5. HPLC methods according to claim 4, it is characterised in that：Per 1g Pinellia Tubers, the dosage of water is 20~50mL；
Preferably, per 1g Pinellia Tubers 50mL water.
6. HPLC methods according to claim 3, it is characterised in that：In step a, per 25ml supernatants 0.1ml phosphoric acid；
And/or the extraction times of ethyl acetate are 5 times.
7. according to the HPLC methods described in claim 3-6 any one, it is characterised in that：The time of the ultrasonic extraction is 15
~120 minutes；Preferably, the time of extraction is 60 minutes.
8. HPLC methods according to claim 3, it is characterised in that：In step c, the specification of the chromatographic column is：Internal diameter
4.6mm, length 250mm, 5 μm of packing material size；Preferable chromatographic column model Inertsil ODS-3 C18 chromatographic columns.
9. HPLC methods according to claim 3, it is characterised in that：In step c, mobile phase is that the phosphoric acid of methanol -0.1% is molten
Liquid (3:97), the phosphoric acid solution of acetonitrile -0.1% (3:Or the phosphoric acid solution of methanol -0.1% (10 97):90).
10. HPLC methods according to claim 3, it is characterised in that：The column temperature of the chromatographic condition is 25~35 DEG C；Stream
Speed is 0.5~0.8mL/min；
Preferably, column temperature is 35 DEG C；Flow velocity is 0.8mL/min.
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| CN107894473B (en) | 2020-06-30 |
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