CN106841467A - The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit - Google Patents
The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit Download PDFInfo
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- CN106841467A CN106841467A CN201710123894.7A CN201710123894A CN106841467A CN 106841467 A CN106841467 A CN 106841467A CN 201710123894 A CN201710123894 A CN 201710123894A CN 106841467 A CN106841467 A CN 106841467A
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- liquid chromatography
- amarogentin
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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Abstract
The invention discloses the high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit；Solve the high-efficiency liquid chromatography method for detecting in the prior art not used for amarogentin in beneficial female biochemistry mixture, and high-efficiency liquid chromatography method for detecting using existing amarogentin causes the undesirable problem of testing result.The present invention includes that (1) prepares need testing solution using beneficial female biochemistry mixture；(2) high performance liquid chromatography detection is carried out, the mobile phase of high performance liquid chromatography detection is 18: 82 first alcohol and water.The present invention has the advantages that testing result more accurate, Detection results are more stablized.
Description
Technical field
The present invention relates to a kind of high-efficiency liquid chromatography method for detecting, and in particular to amarogentin in a kind of female biochemistry mixture of benefit
High-efficiency liquid chromatography method for detecting.
Background technology
Beneficial female biochemistry mixture by motherwort, Radix Angelicae Sinensis, Ligusticum wallichii, peach kernel, baked ginger, Radix Glycyrrhizae (processing) above Six-element medicinal material processing and
Into.There is promoting blood circulation, antalgic, be mainly used in treatment disease that postpartum lochia can't go, abdominal pain due to blood stasis.It is greenish orange yellow
To brown color liquid.Gas is fragrant, and taste is micro- sweet.The female biochemistry mixture of the benefit is mainly used in the livestocks such as horse, ox, sheep, pig, wherein horse, Niu Yong
It is 200-300mL to measure, and sheep, pig consumption are 30-50mL.
Current said preparation record in《Veterinary drug national standard collects --- and veterinary drug provincial standard rises national standard》(second
Volume), indentification by TLC only is carried out to motherwort, Radix Glycyrrhizae, Ligusticum wallichii in its quality standard, without content measuring standard, it is difficult to control
Make its quality, it is ensured that the security of product, validity and quality controllability.
The content of the invention
The technical problems to be solved by the invention are：In the prior art not used for amarogentin in beneficial female biochemistry mixture
High-efficiency liquid chromatography method for detecting, and high-efficiency liquid chromatography method for detecting using existing amarogentin causes testing result to be paid no attention to
The problem thought, it is therefore intended that the high performance liquid chromatography inspection of amarogentin in the female biochemistry mixture of a kind of benefit for solving the above problems is provided
Survey method.
The present invention is achieved through the following technical solutions：
The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit, including：
(1) need testing solution is prepared using beneficial female biochemistry mixture；
(2) high performance liquid chromatography detection is carried out, the mobile phase of high performance liquid chromatography detection is 18: 82 first alcohol and water.
Further, the preparation process of the need testing solution is as follows：
According to beneficial female biochemistry mixture prescription, the female biochemistry mixture of benefit is prepared；5mL is taken in 25mL volumetric flasks, it is dilute with mobile phase
Release to scale, obtain final product.Chromatographic column uses C in the liquid chromatographic detection18Chromatographic column, the Detection wavelength of chromatographic column is 210nm, stream
Speed is 1mLmin-1；Column temperature is 30 DEG C；Sample size is 10 μ L.
In the prior art when the high performance liquid chromatography detection of amarogentin is carried out, due to there are other compositions in medicine,
Other compositions can interfere effect to composition to be measured, thus in different medicines, although composition to be measured is the same, but is applied to
The preprocessing means of one of which medicine are not necessarily suitable another medicine.Also, inventor has found same materials composition
Medicine, when its preparation technology has differences, extreme influence is will also result in final finished, especially for using high-efficient liquid phase color
For spectrum detection, wherein testing result very different when a certain component is detected, thus, above-mentioned factor also results in chromatogram inspection
The poor problem of the effect of survey.
By the optimization of above-mentioned detection method and testing conditions, the shadow that other compositions are detected to amarogentin is effectively prevent
Ring, testing result more accurate, Detection results is more stablized.
Further, also including reference substance solution and negative control solution, the preparation method of the reference substance solution is as follows：
Precision weighs 4.65mg amarogentins reference substance in 50mL volumetric flasks, and quarter is dissolved and be settled to 70% methyl alcohol
Degree, shakes up, and obtains final product 93 μ g/mL amarogentin reference substance solutions；
The preparation method of the negative control solution is as follows：
According to beneficial female biochemistry mixture prescription, other medicinal materials outside peach kernel are removed, be made mixture by formulation and technology, then take 5mL
In 25mL volumetric flasks, scale is diluted to mobile phase, obtained final product.
Preparation technology by optimizing control medicinal material solution and negative control solution of the invention, effectively demonstrates present invention side
The accuracy of method detection.
The present invention compared with prior art, has the following advantages and advantages：
By optimization design of the invention, testing result more accurate, Detection results are made more to stablize.
Brief description of the drawings
Fig. 1 is the chromatogram of the reference substance solution of embodiment 1.
Fig. 2 is the chromatogram of the need testing solution of embodiment 1.
Fig. 3 is the chromatogram of the negative control solution of embodiment 1.
Fig. 4 is methyl alcohol in embodiment 2:Water=20:The chromatogram of need testing solution when 80.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, with reference to embodiment, the present invention is made
Further to describe in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1
A kind of high-efficiency liquid chromatography method for detecting of amarogentin in female biochemistry mixture of benefit, specific detection process is as follows：
(1) preparation of need testing solution：According to beneficial female biochemistry mixture prescription, the female biochemistry mixture of benefit is prepared.5mL is taken in 25mL
In volumetric flask, scale is diluted to mobile phase, obtained final product.The preparation of reference substance solution：Precision weighs the control of 4.65mg amarogentins
Product are dissolved with 70% methyl alcohol and are settled to scale in 50mL volumetric flasks, are shaken up, and obtain final product 93 μ g/mL amarogentin reference substances molten
Liquid.The preparation of negative control solution：According to beneficial female biochemistry mixture prescription, other medicinal materials outside peach kernel are removed, by formulation and technology system
Into mixture, then 5mL is taken in 25mL volumetric flasks, scale is diluted to mobile phase, obtain final product.
(2) high performance liquid chromatography detection is carried out using above-mentioned three kinds of different solution.Wherein, chromatographic column：Global
Chromatography C18(250mm×4.6mm,5μm)；Flow velocity：1mL·min-1；Column temperature：30℃；Sample size：10μL；Inspection
Survey wavelength：210nm.Mobile phase：Methanol-water, methyl alcohol:Water=18:82.
Testing result, as shown in Figure 1-Figure 3：
In test sample chromatogram, there is correspondence at retention time position corresponding to amarogentin reference substance chromatogram main peak
Peak, and good with the separating degree at previous peak, negative sample chromatogram at identical retention time without peak, i.e., it is negative noiseless.
Show that this chromatographic condition specificity is good.
Embodiment 2
The present embodiment is the comparative examples of embodiment 1, and the proportion of composing of mobile phase is different in the present embodiment, specific detection
Process is as follows：
Difference methyl alcohol:Water=20:80 ratio is tried confession as mobile phase using testing conditions same as Example 1
Product solution is detected that testing result is as indicated at 4.While employing methyl alcohol:Water=14:86 are examined as mobile phase
Survey, testing result is：In test sample chromatogram, amarogentin and the separating degree R=1.48 ＜ 1.50 at previous peak are unsatisfactory for HPLC
Basic separation requirement.
Embodiment 3
The present embodiment is examined to the linear relationship of the detection method in embodiment 1, precision, repeatability and stability
Survey, detection method and result are as follows：
Linear relationship is investigated
The accurate μ L of amarogentin reference substance solution 6,8,10,12,14 that draw are injected in liquid chromatograph respectively, the bitter apricot of record
Benevolence glycosides peak area, with integrating peak areas value (Y) as ordinate, reference substance sample size (X) be abscissa draw standard curve, linearly
Regression equation is Y=106.27X+213.45, r=0.9999 (n=5).Result show the sample size of amarogentin 0.558~
With integrating peak areas value in good linear relationship in 1.302 μ g ranges.
Precision test
The μ L of amarogentin reference substance solution 10 are taken, continuous sample introduction 6 times records chromatographic peak peak area, the chromatogram of amarogentin
The RSD of peak-to-peak area is 0.44%.Result shows that instrument precision is good.
Replica test
The same female biochemistry mixture 5mL of batch benefit is taken, 6 parts, need testing solution, sample introduction analysis, record amarogentin peak is prepared
Area, as a result the RSD of amarogentin peak area is 0.51%.Show the repeatability of this method preferably.
Stability test
Beneficial female biochemistry mixture 5mL is taken, need testing solution is prepared.Analyzed respectively at 0,2,4,6,8,10,12h sample introductions, record
Amarogentin peak area, the RSD for calculating peak area is 2.16%.Result shows need testing solution stabilization in 12h.
Meanwhile, the present embodiment is also measured to average recovery, and assay method is：Precision measures beneficial female biochemistry mixture
2.5mL, totally 6 parts, in 25mL volumetric flasks, each precision measures appropriate amarogentin reference substance solution, is prepared by need testing solution
Prepared by method, respectively sample introduction, determines amarogentin content, calculates the rate of recovery.Measurement result is as shown in table 1.
Table 1
By above-mentioned testing result：The stability of preferred scheme of the present invention, repeatability are very excellent, and sample-adding
The RSD values of the rate of recovery reach 2.96, effect highly significant.
Above-described specific embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that and the foregoing is only specific embodiment of the invention, be not intended to limit the present invention
Protection domain, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. all should include
Within protection scope of the present invention.
Claims (4)
1. in a kind of female biochemistry mixture of benefit amarogentin high-efficiency liquid chromatography method for detecting, it is characterised in that including：
(1) need testing solution is prepared using beneficial female biochemistry mixture；
(2) high performance liquid chromatography detection is carried out, the mobile phase of high performance liquid chromatography detection is 18: 82 first alcohol and water.
2. in the female biochemistry mixture of a kind of benefit according to claim 1 amarogentin high-efficiency liquid chromatography method for detecting, its
It is characterised by, the preparation process of the need testing solution is as follows：
According to beneficial female biochemistry mixture prescription, the female biochemistry mixture of benefit is prepared；5mL is taken in 25mL volumetric flasks, is diluted to mobile phase
Scale, obtains final product.
3. in the female biochemistry mixture of a kind of benefit according to claim 1 and 2 amarogentin high-efficiency liquid chromatography method for detecting,
Characterized in that, chromatographic column uses C in the liquid chromatographic detection18Chromatographic column, the Detection wavelength of chromatographic column is 210nm, flow velocity
It is 1mLmin-1；Column temperature is 30 DEG C；Sample size is 10 μ L.
4. in the female biochemistry mixture of a kind of benefit according to claim 1 and 2 amarogentin high-efficiency liquid chromatography method for detecting,
Characterized in that, also including reference substance solution and negative control solution, the preparation method of the reference substance solution is as follows：
Precision weighs 4.65mg amarogentins reference substance in 50mL volumetric flasks, is dissolved with 70% methyl alcohol and is settled to scale, shakes
It is even, obtain final product 93 μ g/mL amarogentin reference substance solutions；
The preparation method of the negative control solution is as follows：
According to beneficial female biochemistry mixture prescription, remove other medicinal materials outside peach kernel, mixture be made by formulation and technology, then take 5mL in
In 25mL volumetric flasks, scale is diluted to mobile phase, obtained final product.
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| CN201710123894.7A CN106841467A (en) | 2017-03-03 | 2017-03-03 | The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit |
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| CN201710123894.7A CN106841467A (en) | 2017-03-03 | 2017-03-03 | The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit |
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Citations (7)
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|---|---|---|---|---|
| JPH06192265A (en) * | 1992-12-25 | 1994-07-12 | Snow Brand Milk Prod Co Ltd | 4,15-dihydrovernodalin |
| WO2004014409A1 (en) * | 2002-08-12 | 2004-02-19 | Herb Valley | Developing method for separating d-amygdalin and neoamygdalin by reversed-phase hplc and optimum conditions for inhibition of racemization of amygdalin |
| CN1515272A (en) * | 2003-01-08 | 2004-07-28 | 江苏康缘药业股份有限公司 | Chinese medicine composition for curing cough, its preparation method and quality control method |
| JP2008037771A (en) * | 2006-08-02 | 2008-02-21 | Hyper Plants Co Ltd | Method for extracting valuable component from eriobotrya japonica seed |
| CN101653491A (en) * | 2009-07-16 | 2010-02-24 | 陈世忠 | Preparation technology and quality control method of preparation containing cassia twig and tuckahoe |
| CN104777249A (en) * | 2015-04-07 | 2015-07-15 | 湖北端正药业股份有限公司 | Method for determining content of effective ingredient amygdalin in loquat leaf cough syrup |
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2017
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Patent Citations (7)
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|---|---|---|---|---|
| JPH06192265A (en) * | 1992-12-25 | 1994-07-12 | Snow Brand Milk Prod Co Ltd | 4,15-dihydrovernodalin |
| WO2004014409A1 (en) * | 2002-08-12 | 2004-02-19 | Herb Valley | Developing method for separating d-amygdalin and neoamygdalin by reversed-phase hplc and optimum conditions for inhibition of racemization of amygdalin |
| CN1515272A (en) * | 2003-01-08 | 2004-07-28 | 江苏康缘药业股份有限公司 | Chinese medicine composition for curing cough, its preparation method and quality control method |
| JP2008037771A (en) * | 2006-08-02 | 2008-02-21 | Hyper Plants Co Ltd | Method for extracting valuable component from eriobotrya japonica seed |
| CN101653491A (en) * | 2009-07-16 | 2010-02-24 | 陈世忠 | Preparation technology and quality control method of preparation containing cassia twig and tuckahoe |
| CN104777249A (en) * | 2015-04-07 | 2015-07-15 | 湖北端正药业股份有限公司 | Method for determining content of effective ingredient amygdalin in loquat leaf cough syrup |
| CN106324117A (en) * | 2016-08-03 | 2017-01-11 | 鲁南厚普制药有限公司 | Quality detection method for dysuria remedying granules |
Non-Patent Citations (3)
| Title |
|---|
| 叶晶晶: "HPLC法测定不同产地桃仁中苦杏仁苷的含量", 《中华中医药学刊》 * |
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