CN105301128B - Detection method of medicine preparation having effects of nourishing blood, relieving restlessness, tranquilizing mind and calming nerves - Google Patents
Detection method of medicine preparation having effects of nourishing blood, relieving restlessness, tranquilizing mind and calming nerves Download PDFInfo
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Abstract
The invention belongs to the field of detection of traditional Chinese medicine preparations and particularly relates to a detection method of a medicine preparation having the effects of nourishing blood, relieving restlessness, tranquilizing mind and calming nerves. According to the detection method, spinosin in mind and nerve tranquilizing tablets can be extracted to a great degree by selecting an extraction solvent, extraction time, an extraction method and the like; the separation effect of the spinosin in the mind and nerve tranquilizing tablets and other chemical components can be best by selecting a chromatographic column, a gradient elution method and the like, and accordingly the spinosin content in the mind and nerve tranquilizing tablets is accurately determined. The detection method is accurate, sensitive, simple and convenient and good in stability and reproducibility, an HPLC chromatogram is good in peak pattern, accordingly the spinosin content in the mind and nerve tranquilizing tablets is accurately determined, and the detection method is beneficial to effective control on the quality of the medicine and improvement of the safety and stability of the medicine in use.
Description
Technical field
The invention belongs to Chinese medicine preparation detection field, and in particular to a kind of medicine acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming
The detection method of thing preparation.
Background technology
Xinshen Ning tablets are by written by Eastern Han Dynasty's holy doctor Zhang Zhongjing《Medical Treasures of the Golden Chamber》In suanzaoren decoctionization cut out.By stir-fry Ziziphi Spinosae
The Six-element such as core, Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata, Radix Glycyrrhizae Chinese medicine is constituted, and is recorded in the national drug standards (WS-10410 (ZD-
0410) 2002-2012Z), with blood-nourishing relieving restlessness, effect of mind tranquilizing and the heart calming, for heart-liver blood deficiency, insomnia and dreamful sleep is irritated and shy,
The diseases such as tired lack of appetite.Xinshen Ning tablets are evident in efficacy, and clinical practice is relatively broad.Wherein Semen Ziziphi Spinosae (parched) be side in monarch drug, play to
Important effect is closed, the quality of the quality of medicinal material that feeds intake, the height of component content directly affect the drug effect of Xinshen Ning tablets.
Semen Ziziphi Spinosae for Rhamnaceae jujube Ziziphi Spinosae dry mature seed, with mind tranquilizing and the heart calming, promote the production of body fluid, tonifying liver mind calming,
Effect of tonifying YIN arresting sweating, is one of traditional tranquillizing and allaying excitement medicine.Principle active component is saponinss and flavonoid in Semen Ziziphi Spinosae
Compound.
《HPLC methods determine spinosin content in Semen Ziziphi Spinosae dispersible tablet》(Asia-Pacific traditional medicine, 2013,9 (7), 41-42),
Disclose herein below：" method：Using HPLC methods, with Diamonsil C18 chromatographic columns (4.6mm × 250mm, 5 μm)；With second
Nitrile (A)-water (0.1% acetic acid) is (B) eluent gradient eluting；Flow velocity 1.0mL/min, column temperature is 25 DEG C, and Detection wavelength is
335nm.As a result：Spinosin relation in the range of 3.36-32.36 μ g/g (r=0.9992) is good, and mean sample recovery rate is
99.23% (n=6)；RSD is 1.51% ".With《HPLC methods determine spinosin content in Semen Ziziphi Spinosae dispersible tablet》Method to the heart
When the content of the spinosin of refreshing peaceful piece is measured, due to Xinshen Ning tablets by Semen Ziziphi Spinosae (parched), Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata,
The Six-element such as Radix Glycyrrhizae Chinese medicine is constituted, and is connected each other between each Chinese medicine, interacts, is influenced each other, in spinosin and Xinshen Ning tablets
Other chemical compositions separating effect it is poor, so as to cause that assay can not be carried out.Therefore,《HPLC methods determine Semen Ziziphi Spinosae
Spinosin content in dispersible tablet》Method be not particularly suited for the assay of spinosin in Xinshen Ning tablets.
Therefore, a kind of content assaying method of spinosin in Xinshen Ning tablets is set up, for the quality of Xinshen Ning tablets is carried out
Control comprehensively significant.
The content of the invention
Therefore, the technical problem to be solved in the present invention is without the content of spinosin in Xinshen Ning tablets in prior art
Assay method, the technical problem for being unfavorable on the whole carrying out the quality of Xinshen Ning tablets comprehensive control, so as to propose a kind of tool
There are blood-nourishing relieving restlessness, the detection method of the pharmaceutical preparation of mind tranquilizing and the heart calming effect.
To solve above-mentioned technical problem, the present invention is achieved through the following technical solutions：
The present invention provides a kind of detection method of the pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming, the medicine
The crude drug of preparation is consisted of：Semen Ziziphi Spinosae (parched), Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata, Radix Glycyrrhizae；
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, take 0.2 weight portion～0.8 weight
Part, it is accurately weighed, in putting conical flask with cover, precision add 50%～100% methanol or the parts by volume of 50%～100% ethanol 15～
35 parts by volume, weighed weight, ultrasound 5～50 minutes or is heated to reflux 5～50 minutes, lets cool, weighed weight, with 50%～
100% methanol or 50%～100% ethanol supply the weight of less loss, shake up, and filter, and take subsequent filtrate, obtain final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise 0.005～0.015mg/mL of element；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with water-
0.1% glacial acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min,
A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% →
23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：
B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：
90%；Detection wavelength 335nm；20 DEG C～30 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 8～12, high performance liquid chromatograph is injected, determine；
The weight portion is g/mL with the relation of parts by volume.
Preferably, in the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention,
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, take 0.4 weight portion～0.6 weight
Part, accurately weighed, in putting conical flask with cover, precision adds 65%～75% methanol or parts by volume～30 of 65%～75% ethanol 20
Parts by volume, weighed weight, ultrasound 8～12 minutes or is heated to reflux 8～12 minutes, lets cool, weighed weight, with 65%～75% first
Alcohol or 65%～75% ethanol supply the weight of less loss, shake up, and filter, and take subsequent filtrate, obtain final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise 0.008～0.012mg/mL of element；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with water-
0.1% glacial acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min,
A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% →
23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：
B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：
90%；Detection wavelength 335nm；23 DEG C～27 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 9～11, high performance liquid chromatograph is injected, determine.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In,
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.5 weight portion is taken, precision claims
Fixed, in putting conical flask with cover, precision adds 70% methanol or the parts by volume of 70% ethanol 25, weighed weight, ultrasound 10 minutes or adds
Hot reflux 10 minutes, lets cool, weighed weight, and with 70% methanol or 70% ethanol the weight of less loss is supplied, and shakes up, and filters, and takes continuous
Filtrate, obtains final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise element 0.010mg/mL；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with water-
0.1% glacial acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min,
A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% →
23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：
B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：
90%；Detection wavelength 335nm；25 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 10, high performance liquid chromatograph is injected, determine.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the chromatographic column is selected from 4.6mm × 250mm, 5 μm of Perkin Elmer C18 or 4.6 × 250mm, 5 μm of Agilent
C18 or 4.6 × 250mm, 5 μm of Inertsil ODS-3.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, also including the step of the preparation of following negative controls solution：
The crude drug of the negative controls is consisted of：Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata, Radix Glycyrrhizae；
Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.2 weight portion～0.8 weight portion is taken, it is accurately weighed, put tool plug
In conical flask, precision adds 50%～100% methanol or parts by volume～35 parts by volume of 50%～100% ethanol 15, weighed weight,
Ultrasound 5～50 minutes is heated to reflux 5～50 minutes, lets cool, weighed weight, with 50%～100% methanol or 50%～100%
Ethanol supplies the weight of less loss, shakes up, and filters, and takes subsequent filtrate, obtains final product the negative controls solution.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In,
Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.4 weight portion～0.6 weight portion is taken, it is accurately weighed, put tool plug
In conical flask, precision adds 65%～75% methanol or parts by volume～30 parts by volume of 65%～75% ethanol 20, weighed weight to surpass
Sound 8～12 minutes is heated to reflux 8～12 minutes, lets cool, weighed weight, with 65%～75% methanol or 65%～75% ethanol
The weight of less loss is supplied, is shaken up, filtered, take subsequent filtrate, obtain final product the negative controls solution.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, it is the step of the preparation of the negative controls solution：Negative controls to be measured are taken, it is accurately weighed, it is finely ground, take 0.5 weight
Part, accurately weighed, in putting conical flask with cover, precision adds 70% methanol or the parts by volume of 70% ethanol 25, weighed weight, ultrasound 10
Minute is heated to reflux 10 minutes, lets cool, weighed weight, and with 70% methanol or 70% ethanol the weight of less loss is supplied, and shakes up, mistake
Filter, takes subsequent filtrate, obtains final product the negative controls solution.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the high performance liquid chromatograph is selected from Japanese Shimadzu, Agilent 1100 or Agilent 1260.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the crude drug of the pharmaceutical preparation is consisted of：The crude drug of the pharmaceutical preparation is consisted of：Semen Ziziphi Spinosae (parched) 220-280 weight
It is part, Radix Polygalae 140-190 weight portion, Poria 140-190 weight portions, Fructus Gardeniae 50-110 weight portions, Massa Medicata Fermentata 50-110 weight portions, sweet
Careless 50-110 weight portions；
The crude drug of the negative controls is consisted of：Radix Polygalae 140-190 weight portion, Poria 140-190 weight portions, Fructus Gardeniae
50-110 weight portions, Massa Medicata Fermentata 50-110 weight portions, Radix Glycyrrhizae 50-110 weight portions.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the crude drug of the pharmaceutical preparation is consisted of：The weight portion of Semen Ziziphi Spinosae (parched) 250, the weight portion of Radix Polygalae 167, the weight portion of Poria 167,
The weight portion of Fructus Gardeniae 83, the weight portion of Massa Medicata Fermentata 83, the weight portion of Radix Glycyrrhizae 83；
The crude drug of the negative controls is consisted of：The weight portion of Radix Polygalae 167, the weight portion of Poria 167, the weight of Fructus Gardeniae 83
Part, the weight portion of Massa Medicata Fermentata 83, the weight portion of Radix Glycyrrhizae 83.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the pharmaceutical preparation be tablet, capsule, pill, granule, honey refining pill, slow releasing preparation, quick releasing formulation, controlled release preparation,
Oral liquid or ejection preparation.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the pharmaceutical preparation is prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Semen Ziziphi Spinosae (parched), Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, 3 are decocted for the first time little
When, second decoction 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, added customary adjuvant, make clinic according to common process
Acceptable dosage form；
The negative controls are prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, decocted 3 hours for the first time, second
Decoct 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, added customary adjuvant, make clinic according to common process
Acceptable dosage form.
It is further preferred that the detection method of the above-mentioned pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming of the present invention
In, the pharmaceutical preparation is tablet, and the tablet is prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Semen Ziziphi Spinosae (parched), Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, 3 are decocted for the first time little
When, second decoction 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, add right amount of auxiliary materials, pelleting, add magnesium stearate to fit
Amount, mixes, and is dried, and tabletted, coating obtains final product tablet.
Technical scheme has the advantage that：
The present invention with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, by selective extraction solvent,
Extraction time, extracting method etc. so that the spinosin in Xinshen Ning tablets is farthest extracted；By select chromatographic column,
Method of gradient elution etc. so that the spinosin in Xinshen Ning tablets is best with the separating effect of other chemical compositions, so as to standard
Really the content of the spinosin in Xinshen Ning tablets is measured.The detection method is accurate, sensitive, easy, stability and weight
Existing property is good, and HPLC chromatogram peak type is good, so as to be measured to the content of the spinosin in Xinshen Ning tablets exactly, favorably
It control effectively in the quality to the medicine, is favorably improved the safety and stability that the medicine is used.
Description of the drawings
In order to be illustrated more clearly that the specific embodiment of the invention or technical scheme of the prior art, below will be to concrete
The accompanying drawing to be used needed for embodiment or description of the prior art is briefly described.It should be evident that below in description
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, can be with according to these other accompanying drawings of accompanying drawings acquisition.
Fig. 1 is the high-efficient liquid phase chromatogram of Xinshen Ning tablets negative controls solution in experimental example of the present invention 1；
Fig. 2 is the high-efficient liquid phase chromatogram of Xinshen Ning tablets need testing solution in experimental example of the present invention 1；
Fig. 3 is the high-efficient liquid phase chromatogram of spinosin reference substance solution in experimental example of the present invention 1；
Fig. 4 is the high-efficient liquid phase chromatogram of spinosin reference substance solution in experimental example of the present invention 2；
Fig. 5 is the high-efficient liquid phase chromatogram of Xinshen Ning tablets need testing solution in experimental example of the present invention 2.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described enforcement
Example is a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Experimental example 1
1 instrument and material
Agilent1260 high performance liquid chromatographs, evaporate photodetector detector；VWD detectors；The medical numbers of KQ-500DE
Control ultrasonic cleaner；The a ten thousandth electronic analytical balances of AE 2,400, Switzerland's prunus mume (sieb.) sieb.et zucc. Teller.
Spinosin reference substance (lot number 111869-201203) is bought by National Institute for Food and Drugs Control；Acetonitrile is (beautiful
State Fisher), methanol (U.S. Fisher) be chromatographically pure；Methanol (the good Xinghua work glass apparatus Trade Co., Ltd. in Tianjin), ice
Acetic acid (Tianjin recovery development in science and technology company limited) is pure, the water of analysis (three-level reverse osmosis legal system obtains purified water).
Xinshen Ning tablets (lot number 492043), Xinshen Ning tablets negative controls, prepare used by Xinshen Ning tablets negative controls
Raw material is provided by Jingfukang Pharmaceutical Group Co., Ltd., by Jingfukang Pharmaceutical Group Co., Ltd.'s engineer's TCD identification Shi Jian
It is set to genuine piece.Xinshen Ning tablets according to embodiment 1 method prepare, Xinshen Ning tablets negative controls according to embodiment 2 method system
It is standby.
2.2.1 chromatographic condition
Using Perkin Elmer C18 chromatographic columns (4.6mm × 250mm, 5 μm)；A (acetonitrile)-B (0.1% glacial acetic acid) is
Mobile phase, online gradient elution, 0-15min-25min-30min-33min-37min, A phase is 10%-17%-23%-35%-
10%-10%；Detection wavelength：335nm；Column temperature：25℃；Flow velocity：1.0mL/min；Sampling volume：10μL.
2.2.2 the preparation of reference substance solution
Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes the reference substance containing spinosin 0.01mg/mL
Solution.
2.2.3 the preparation of need testing solution
Take Xinshen Ning tablets several pieces, remove coating, it is accurately weighed, it is finely ground, take about 0.5g, it is accurately weighed, put conical flask with cover
In, precision adds 70% methanol 25mL, weighed weight, ultrasound 10 minutes to let cool, and weighed weight supplies less loss with 70% methanol
Weight, shake up, filter, take subsequent filtrate and obtain final product.
2.2.4 the preparation of negative controls solution
By negative sample of the flavour of a drug proportions in prescription without Semen Ziziphi Spinosae medical material, prepare according to " 2..2.3 " item lower section method
Negative controls.
2.2.5 specificity experiment
By above-mentioned experiment condition, respectively negative controls solution, need testing solution and reference substance solution are injected into liquid phase color
Spectrometer is determined, and gained high-efficient liquid phase chromatogram is shown in respectively Fig. 1, Fig. 2 and Fig. 3.
As shown in Figure 1, under the chromatographic condition, negative controls solution is noiseless.
2.2.6 linear relationship is investigated
Precision weighs reference substance in right amount, plus methanol makes the reference substance liquid containing spinosin 0.053424mg/mL, using again
Series mass strength solution is made than dilution method, the concentration for making spinosin is respectively 0.026712mg/mL, 0.013356mg/
ML, 0.006678mg/mL, 0.003339mg/mL.HPLC analyses are carried out according to chromatographic condition under " 2.2.1 " item.With spinosin
Peak area Y standard curve drawn to concentration X of spinosin obtain regression equation Y=20043X+4.4708, r=0.9999 (n
=5).
As a result show, the linear relationship in the range of 3.339-53.424 μ g/mL of the spinosin in Xinshen Ning tablets is good.
2.2.7 Precision Experiment
The reference substance solution that content is 0.013356mg/mL is taken, according to the chromatographic condition under " 2.2.1 " item, repeats sample introduction 6
It is secondary, each chromatographic peak area is recorded, calculate RSD values.
As a result show, the spinosin RSD values in Xinshen Ning tablets are 0.75%.That is, the detection method precision is good.
2.2.8 repeated experiment
Precision weighs same lot number Xinshen Ning tablets (lot number 492043), by legal system available test sample solution 6 below " 2.2.2 " item
Part, determine by chromatographic condition under " 2.2.1 " item, record chromatographic peak area.
As a result show, the average content of the spinosin in Xinshen Ning tablets is 0.1623mg/ pieces, and RSD is 1.46% (n=
6).That is, the detection method favorable reproducibility.
2.2.9 stability experiment
The need testing solution prepared according to " 2.2.2 " item lower section method is taken, 0,2,4,6,8,10,12h is entered after the production respectively
The μ L of sample 10, record chromatographic peak area.
As a result show, the spinosin chromatographic peak area RSD values in Xinshen Ning tablets are 1.46%.That is, need testing solution exists
12h internal stabilities are good.
2.2.10 average recovery experiment
Precision weighs 9 parts of Xinshen Ning tablets (lot number 492043) for determining spinosin (0.1530mg/ pieces) content, accurate
Weighed 0.25g, adds a certain amount of reference substance, according to " 2.2.2 " item lower section legal system available test sample solution, by color under " 2.2.1 " item
Spectral condition is measured, and with absolute mass fraction in need testing solution average recovery is calculated, and specific experiment the results are shown in Table 2.
Spinosin average recovery experimental result (n=9) of table 2
As shown in Table 2, the spinosin average recovery rate in Xinshen Ning tablets is that 100.91%, RSD values are 1.36%.
2.2.10 the determination of quantitative limit
The reference substance solution dilution of least concentration in standard curve working solution is taken, is entered by the chromatographic condition under " 2.2.1 " item
Row detection, sample size is 10 μ L, then constantly presses multiple dilutions, is determined.
As a result show, the spinosin concentration in Xinshen Ning tablets is 10 for the solution signal to noise ratio of 0.001166667mg/mL:
1, it is determined that being quantitatively limited to 11.66667ng.
2.2.11 the determination of test limit
The reference substance solution dilution of least concentration in standard curve working solution is taken, is entered by the chromatographic condition under " 2.2.1 " item
Row detection, sample size is 10 μ L, then constantly presses multiple dilutions, is determined.
As a result show, the solution signal to noise ratio that spinosin concentration is 0.000875mg/mL of measuring in Xinshen Ning tablets is 3:
1, it is determined that detection is limited to 8.75ng.
2.2.12 sample size is determined
By above-mentioned chromatographic condition determine Jingfukang Pharmaceutical Group Co., Ltd.'s Xinshen Ning tablets (lot number 392,170 030,
492009 029,492016,492043) and on the market certain producer Xinshen Ning tablets (lot number 140519,140802,140804) in
Spinosin, specific experiment the results are shown in Table 3.
The sample size measurement result of table 3
| Sample lot number | Spinosin content (mg/ pieces) |
| 392170 | 0.1598 |
| 492009 | 0.1820 |
| 492016 | 0.1597 |
| 492043 | 0.1530 |
| 140802 | 0.1237 |
| 140804 | 0.1313 |
| 140519 | 0.1482 |
As shown in Table 3, the detection method of the pharmaceutical preparation that the present invention is acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming, can be with standard
Really the content of the spinosin in Xinshen Ning tablets is measured, and then the quality to the medicine is controlled.
In sum, the detection method of the pharmaceutical preparation that the present invention is acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming, accurate, spirit
Quick, easy, stability and repeatability are good, and HPLC chromatogram peak type is good, so as to exactly to the spinosin in Xinshen Ning tablets
Content be measured, be conducive to controling effectively the quality of the medicine, be favorably improved the safety that the medicine is used
And stability.
Experimental example 2
Comparative example 1
This comparative example is differed only in 4.6 × 250mm with embodiment 3, and 5 μm of Agilent C18 are chromatographic column, its
Remaining experiment condition and operating procedure are same as Example 3.
As a result show, the separating effect of the spinosin in this comparative example in Xinshen Ning tablets is not so good as the Xinshen Ning tablets of embodiment 3
In spinosin good separating effect, retention time is moderate.
Comparative example 2
This comparative example is differed only in 4.6 × 250mm with embodiment 3, and 5 μm of Inertsil ODS-3 are chromatograph
Post, remaining experiment condition and operating procedure it is same as Example 3.
As a result show, the separating effect of the spinosin in this comparative example in Xinshen Ning tablets is not so good as the Xinshen Ning tablets of embodiment 3
In spinosin good separating effect, retention time is moderate.
Comparative example 3
The present embodiment is differed only in embodiment 3, in the preparation of need testing solution, is heated to reflux 10 minutes, remaining
Experiment condition and operating procedure are same as Example 3.
As a result show, the mind of content and embodiment 3 measure of the spinosin in the Xinshen Ning tablets that this comparative example is determined
Content in peaceful piece is identical.
Comparative example 4
This comparative example is differed only in embodiment 3, and in the preparation of need testing solution, precision adds 50% ethanol
25mL, with 50% ethanol the weight of less loss is supplied, and remaining experiment condition and operating procedure are same as Example 3.
As a result show, the content of the spinosin in the Xinshen Ning tablets that this comparative example is determined is than the mind that embodiment 3 is determined
Content in peaceful piece is low.
Comparative example 5
This comparative example is differed only in embodiment 3, and in the preparation of need testing solution, precision adds 50% methanol
25mL, with 50% methanol the weight of less loss is supplied, and remaining experiment condition and operating procedure are same as Example 3.
As a result show, the content of the spinosin in the Xinshen Ning tablets that this comparative example is determined is than the mind that embodiment 3 is determined
Content in peaceful piece is low.
Comparative example 6
This comparative example is differed only in embodiment 3, and in the preparation of need testing solution, precision adds 100% ethanol
25mL, with 100% ethanol the weight of less loss is supplied, and remaining experiment condition and operating procedure are same as Example 3.
As a result show, the content of the spinosin in the Xinshen Ning tablets that this comparative example is determined is than the mind that embodiment 3 is determined
Content in peaceful piece is low.
Comparative example 7
This comparative example is differed only in embodiment 3, and in the preparation of need testing solution, precision adds 100% methanol
25mL, with 100% methanol the weight of less loss is supplied, and remaining experiment condition and operating procedure are same as Example 3.
As a result show, the content of the spinosin in the Xinshen Ning tablets that this comparative example is determined is than the mind that embodiment 3 is determined
Content in peaceful piece is low.
Comparative example 8
This comparative example is differed only in embodiment 3, in the preparation of need testing solution, ultrasound 20 minutes, and remaining experiment
Condition and operating procedure are same as Example 3.
As a result show, the mind of content and embodiment 3 measure of the spinosin in the Xinshen Ning tablets that this comparative example is determined
Content in peaceful piece is identical.
Comparative example 9
This comparative example is differed only in embodiment 3, in the preparation of need testing solution, ultrasound 30 minutes, and remaining experiment
Condition and operating procedure are same as Example 3.
As a result show, the mind of content and embodiment 3 measure of the spinosin in the Xinshen Ning tablets that this comparative example is determined
Content in peaceful piece is identical.
Comparative example 10
This comparative example is differed only in embodiment 3, in the preparation of need testing solution, ultrasound 45 minutes, and remaining experiment
Condition and operating procedure are same as Example 3.
As a result show, the mind of content and embodiment 3 measure of the spinosin in the Xinshen Ning tablets that this comparative example is determined
Content in peaceful piece is identical.
Comparative example 11
This comparative example is differed only in embodiment 3, with Diamonsil C18 chromatographic columns (4.6mm × 250mm, 5 μ
m)；With acetonitrile (A)-water (0.1% acetic acid) (B) as eluent gradient eluting；Gradient elution is carried out according to following program：0min,
A：B is 19%：81%；0min-5min, A：B is 19%：91% → 23%：77%；15min, A：B is 23%：77%；
15min-25min, A：B is 23%：77% → 70%：30%；25min, A：B is 70%：30%；25min-35min, A：B is
70%：30% → 90%：10%；30min, A：B is 90%：10%；35min-40min, A：B is 90%：10% → 100%：
0%；40min, A：B is 10%：90%, remaining experiment condition and operating procedure it is same as Example 3.
Specific experiment result is as shown in Figure 4 and Figure 5.
From Fig. 4 and Fig. 5, the chromatographic peak of other chemical compositions in Xinshen Ning tablets has dry to the chromatographic peak of spinosin
Disturb, spinosin is poor with the separating effect of other chemical compositions, so as to cause that assay can not be carried out.Therefore, comparative example
11 method cannot be used for determining the content of the spinosin in Xinshen Ning tablets.
Embodiment 1The preparation of Xinshen Ning tablets
【Prescription】Semen Ziziphi Spinosae (parched) 250g, Radix Polygalae 167g, Poria 167g, Fructus Gardeniae 83g, Massa Medicata Fermentata 83g, Radix Glycyrrhizae 83g.
【Preparation method】The tablet is prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Semen Ziziphi Spinosae (parched), Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, 3 are decocted for the first time little
When, second decoction 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, add right amount of auxiliary materials, pelleting, add magnesium stearate to fit
Amount, mixes, and is dried, and tabletted, coating obtains final product tablet.
Embodiment 2The preparation of Xinshen Ning tablets negative controls
【Prescription】Semen Ziziphi Spinosae (parched) 250g, Radix Polygalae 167g, Poria 167g, Fructus Gardeniae 83g, Massa Medicata Fermentata 83g, Radix Glycyrrhizae 83g.
【Preparation method】The tablet is prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, decocted 3 hours for the first time, second
Decoct 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, add right amount of auxiliary materials, pelleting, add magnesium stearate to fit
Amount, mixes, and is dried, and tabletted, coating obtains final product tablet.
Embodiment 3
The present embodiment has blood-nourishing relieving restlessness, the detection method of the pharmaceutical preparation of mind tranquilizing and the heart calming effect, and the detection method includes
The following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.5g is taken, it is accurately weighed, put tool
In plug conical flask, precision adds 70% methanol 25mL, weighed weight, ultrasound 10 minutes to let cool, and weighed weight uses 70% methanol
The weight of less loss is supplied, is shaken up, filtered, take subsequent filtrate, obtained final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise element 0.010mg/mL；
(3) preparation of negative controls solution：Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.5g is taken, precision claims
Fixed, in putting conical flask with cover, precision adds 70% methanol or ethanol 25mL, weighed weight, ultrasound or is heated to reflux 10 minutes, puts
Cold, weighed weight supplies the weight of less loss with 70% methanol or ethanol, shakes up, and filters, and takes subsequent filtrate, obtains final product；
(4) chromatographic condition：With 4.6mm × 250mm, 5 μm of Perkin Elmer C18 are chromatographic column, with acetonitrile as flowing
Phase A, with the glacial acetic acid of water -0.1% as Mobile phase B, according to following program gradient elution is carried out：0min, A：B is 10%：90%；
0min-15min, A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is
17%：83% → 23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：
65%；30min, A：B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min,
A：B is 10%：90%；Detection wavelength 335nm；25 DEG C of column temperature；Flow velocity 1.0mL/min；
(5) it is accurate respectively to draw need testing solution, reference substance solution, the μ L of negative controls solution 10, inject efficient liquid phase
Chromatograph, determines.
Embodiment 4
The present embodiment has blood-nourishing relieving restlessness, the detection method of the pharmaceutical preparation of mind tranquilizing and the heart calming effect, and the detection method includes
The following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.4g is taken, it is accurately weighed, put tool
In plug conical flask, precision adds 75% methanol 20mL, weighed weight, ultrasound 8 minutes to let cool, weighed weight, mended with 75% methanol
The weight of sufficient less loss, shakes up, and filters, and takes subsequent filtrate, obtains final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise element 0.008mg/mL；
(3) preparation of negative controls solution：Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.4g～0.6g is taken,
Accurately weighed, in putting conical flask with cover, precision adds 75% methanol 20mL, and weighed weight, ultrasound 8 minutes lets cool, weighed heavy
Amount, with 75% methanol the weight of less loss is supplied, and is shaken up, and is filtered, and takes subsequent filtrate, is obtained final product；
(4) chromatographic condition：4.6mm × 250mm, 5 μm of Perkin Elmer C18 are chromatographic column, with acetonitrile as mobile phase
A, with the glacial acetic acid of water -0.1% as Mobile phase B, according to following program gradient elution is carried out：0min, A：B is 10%：90%；
0min-15min, A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is
17%：83% → 23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：
65%；30min, A：B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min,
A：B is 10%：90%；Detection wavelength 335nm；27 DEG C of column temperature；Flow velocity 1.0mL/min；
(5) it is accurate respectively to draw need testing solution, reference substance solution, the μ L of negative controls solution 11, inject efficient liquid phase
Chromatograph, determines.
Embodiment 5
The present embodiment has blood-nourishing relieving restlessness, the detection method of the pharmaceutical preparation of mind tranquilizing and the heart calming effect, and the detection method includes
The following assay step to spinosin：
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.6g is taken, it is accurately weighed, put tool
In plug conical flask, precision adds 65% ethanol 30mL, weighed weight, ultrasound 12 minutes to let cool, and weighed weight uses 65% ethanol
The weight of less loss is supplied, is shaken up, filtered, take subsequent filtrate, obtained final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing this skin
The reference substance solution of promise element 0.012mg/mL；
(3) preparation of negative controls solution：Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.4g～0.6g is taken,
Accurately weighed, in putting conical flask with cover, precision adds 65% ethanol 30mL, weighed weight, ultrasound or is heated to reflux 8～12 points
Clock, lets cool, weighed weight, and with 65% ethanol the weight of less loss is supplied, and shakes up, and filters, and takes subsequent filtrate, obtains final product；
(4) chromatographic condition：4.6mm × 250mm, 5 μm of Perkin Elmer C18 are chromatographic column, with acetonitrile as mobile phase
A, with the glacial acetic acid of water -0.1% as Mobile phase B, according to following program gradient elution is carried out：0min, A：B is 10%：90%；
0min-15min, A：B is 10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is
17%：83% → 23%：77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：
65%；30min, A：B is 35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min,
A：B is 10%：90%；Detection wavelength 335nm；23 DEG C of column temperature；Flow velocity 1.0mL/min；
(5) it is accurate respectively to draw need testing solution, reference substance solution, the μ L of negative controls solution 9, inject high-efficient liquid phase color
Spectrometer, determines.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. it is a kind of with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, it is characterised in that the medicine system
The crude drug of agent is consisted of：Semen Ziziphi Spinosae (parched), Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata, Radix Glycyrrhizae；
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.2 weight portion～0.8 weight portion is taken,
Accurately weighed, in putting conical flask with cover, precision adds 50%～100% methanol or parts by volume～35 of 50%～100% ethanol 15
Parts by volume, weighed weight, ultrasound 5～50 minutes or is heated to reflux 5～50 minutes, lets cool, weighed weight, with 50%～100%
Methanol or 50%～100% ethanol supply the weight of less loss, shake up, and filter, and take subsequent filtrate, obtain final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing spinosin
The reference substance solution of 0.005～0.015mg/mL；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with the ice of water -0.1%
Acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min, A：B is
10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% → 23%：
77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：B is
35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：90%；Inspection
Survey wavelength 335nm；20 DEG C～30 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 8～12, high performance liquid chromatograph is injected, determine；
The weight portion is g/mL with the relation of parts by volume.
2. it is according to claim 1 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, its feature
It is,
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.4 weight portion～0.6 weight portion is taken,
Accurately weighed, in putting conical flask with cover, precision adds 65%～75% methanol or parts by volume～30 body of 65%～75% ethanol 20
Product part, weighed weight, ultrasound 8～12 minutes or is heated to reflux 8～12 minutes, lets cool, weighed weight, with 65%～75% methanol
Or 65%～75% ethanol supply the weight of less loss, shake up, filter, take subsequent filtrate, obtain final product；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing spinosin
The reference substance solution of 0.008～0.012mg/mL；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with the ice of water -0.1%
Acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min, A：B is
10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% → 23%：
77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：B is
35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：90%；Inspection
Survey wavelength 335nm；23 DEG C～27 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 9～11, high performance liquid chromatograph is injected, determine.
3. it is according to claim 2 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, its feature
It is,
The detection method includes the following assay step to spinosin：
(1) preparation of need testing solution：Pharmaceutical preparation to be measured is taken, it is accurately weighed, it is finely ground, 0.5 weight portion is taken, it is accurately weighed, put
In conical flask with cover, precision adds 70% methanol or the parts by volume of 70% ethanol 25, weighed weight, ultrasound 10 minutes or is heated to reflux
10 minutes, let cool, weighed weight, with 70% methanol or 70% ethanol the weight of less loss is supplied, shake up, filter, take subsequent filtrate, i.e.,
；
(2) preparation of reference substance solution：Precision weighs spinosin reference substance in right amount, plus appropriate methanol, makes containing spinosin
The reference substance solution of 0.010mg/mL；
(3) chromatographic condition：With 4.6mm × 250mm, 5 μm of C18 is chromatographic column, with acetonitrile as mobile phase A, with the ice of water -0.1%
Acetic acid is Mobile phase B, and according to following program gradient elution is carried out：0min, A：B is 10%：90%；0min-15min, A：B is
10%：90% → 17%：83%；15min, A：B is 17%：83%；15min-25min, A：B is 17%：83% → 23%：
77%；25min, A：B is 23%：77%；25min-30min, A：B is 23%：77% → 35%：65%；30min, A：B is
35%：65%；30min-33min, A：B is 35%：65% → 10%：90%；33min-37min, A：B is 10%：90%；Inspection
Survey wavelength 335nm；25 DEG C of column temperature；Flow velocity 1.0mL/min；
(4) it is accurate respectively to draw need testing solution and the μ L of reference substance solution 10, high performance liquid chromatograph is injected, determine.
4. according to any one of claim 1-3 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection side
Method, it is characterised in that
The chromatographic column is selected from 4.6mm × 250mm, 5 μm of Perkin Elmer C18 or 4.6 × 250mm, 5 μm of Agilent
C18 or 4.6 × 250mm, 5 μm of Inertsil ODS-3.
5. according to any one of claim 1-3 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection side
Method, it is characterised in that also including the step of the preparation of following negative controls solution：
The crude drug of the negative controls is consisted of：Radix Polygalae, Poria, Fructus Gardeniae, Massa Medicata Fermentata, Radix Glycyrrhizae；
Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.2 weight portion～0.8 weight portion is taken, it is accurately weighed, put tool plug taper
In bottle, precision adds 50%～100% methanol or parts by volume～35 parts by volume of 50%～100% ethanol 15, weighed weight, ultrasound
5～50 minutes are heated to reflux 5～50 minutes, let cool, weighed weight, with 50%～100% methanol or 50%～100% ethanol
The weight of less loss is supplied, is shaken up, filtered, take subsequent filtrate, obtain final product the negative controls solution.
6. it is according to claim 5 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, its feature
It is to be the step of the preparation of the negative controls solution：
Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.4 weight portion～0.6 weight portion is taken, it is accurately weighed, put tool plug taper
In bottle, precision adds 65%～75% methanol or parts by volume～30 parts by volume of 65%～75% ethanol 20, weighed weight, ultrasound 8
～12 minutes are heated to reflux 8～12 minutes, let cool, weighed weight, are mended with 65%～75% methanol or 65%～75% ethanol
The weight of sufficient less loss, shakes up, and filters, and takes subsequent filtrate, obtains final product the negative controls solution.
7. it is according to claim 6 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, its feature
It is to be the step of the preparation of the negative controls solution：
Negative controls to be measured are taken, it is accurately weighed, it is finely ground, 0.5 weight portion is taken, accurately weighed, in putting conical flask with cover, precision adds
Enter 70% methanol or the parts by volume of 70% ethanol 25, weighed weight or is heated to reflux 10 minutes ultrasound 10 minutes, lets cool, weighed heavy
Amount, with 70% methanol or 70% ethanol the weight of less loss is supplied, and is shaken up, and is filtered, and takes subsequent filtrate, obtains final product the negative controls molten
Liquid.
8. it is according to claim 5 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection method, its feature
It is,
The crude drug of the pharmaceutical preparation is consisted of：Semen Ziziphi Spinosae (parched) 220-280 weight portions, Radix Polygalae 140-190 weight portion, Poria
140-190 weight portions, Fructus Gardeniae 50-110 weight portions, Massa Medicata Fermentata 50-110 weight portions, Radix Glycyrrhizae 50-110 weight portions；
The crude drug of the negative controls is consisted of：Radix Polygalae 140-190 weight portion, Poria 140-190 weight portions, Fructus Gardeniae 50-
110 weight portions, Massa Medicata Fermentata 50-110 weight portions, Radix Glycyrrhizae 50-110 weight portions.
9. according to any one of claim 1-3 with blood-nourishing relieving restlessness, mind tranquilizing and the heart calming act on pharmaceutical preparation detection side
Method, it is characterised in that
The pharmaceutical preparation is tablet, capsule, pill, granule, slow releasing preparation, quick releasing formulation, controlled release preparation, liquid oral
Preparation or ejection preparation.
10. the detection method of the pharmaceutical preparation acted on blood-nourishing relieving restlessness, mind tranquilizing and the heart calming according to claim 5, it is special
Levy and be, the pharmaceutical preparation is prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Semen Ziziphi Spinosae (parched), Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, decocted 3 hours for the first time, the
Secondary to decoct 2 hours, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, added customary adjuvant, clinic is made according to common process can connect
The dosage form received；
The negative controls are prepared by following methods：
(1) Radix Glycyrrhizae and the Massa Medicata Fermentata of selected weight portion are taken, is crushed, sieved, mixed, obtain fine powder；
(2) Fructus Gardeniae, Radix Polygalae and the Poria of selected weight portion are taken, is added water to cook twice, decocted 3 hours for the first time, second decoction 2
Hour, collecting decoction, filtration, filtrate is concentrated into the clear paste that 50 DEG C of relative densities are 1.05-1.20；
(3) fine powder is added into the clear paste, is mixed, added customary adjuvant, clinic is made according to common process can connect
The dosage form received.
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| HPLC-MS-MS法同时测定酸枣仁分散片中酸枣仁皂苷A、酸枣仁皂苷B、斯皮诺素的含量;马桂劼等;《食品科学》;20131231;第34卷(第22期);150－153 * |
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