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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
liquid chromatography
amarogentin
mixture
detecting
female biochemistry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710123894.7A
Other languages
Chinese (zh)
Inventor
潘春晖
张会峰
杨琼
雍玲
刘涛
张煊
任园琴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SICHUAN DECHENG ANIMAL HEALTH PRODUCTS Co Ltd
Original Assignee
SICHUAN DECHENG ANIMAL HEALTH PRODUCTS Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SICHUAN DECHENG ANIMAL HEALTH PRODUCTS Co Ltd filed Critical SICHUAN DECHENG ANIMAL HEALTH PRODUCTS Co Ltd
Priority to CN201710123894.7A priority Critical patent/CN106841467A/en
Publication of CN106841467A publication Critical patent/CN106841467A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/74Optical detectors
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8624Detection of slopes or peaks; baseline correction
    • G01N30/8631Peaks
    • G01N30/8634Peak quality criteria

Landscapes

  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Quality & Reliability (AREA)
  • Engineering & Computer Science (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

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

The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit
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.
CN201710123894.7A 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 Pending CN106841467A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
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

Publications (1)

Publication Number Publication Date
CN106841467A true CN106841467A (en) 2017-06-13

Family

ID=59137903

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710123894.7A Pending 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

Country Status (1)

Country Link
CN (1) CN106841467A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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》 *
国家药典委员会: "《中华人民共和国药典2015年版一部》", 30 June 2015, 中国医药科技出版社 *
国家食品药品监督管理局: "复方斯亚旦生发酊", 《中国药品标准》 *

Similar Documents

Publication Publication Date Title
CN101961430B (en) Quality analysis method of compound Ganmaoling tablets
CN105842373A (en) Method for establishing fingerprint of flos lonicerae medicinal preparation
CN106841450A (en) It is a kind of at the same determine Chinese herbaceous peony in 9 kinds of HPLC methods of monomeric compound
CN105353063B (en) Compound cold drug stream livering ingredient standard finger-print and construction method, application
CN104678031B (en) High performance liquid chromatography detects the method for atractyloside and/or earboxyatractylosida
CN108459090B (en) Quality control method of Jichuan decoction composition
CN106053658A (en) Burned Rhizoma drynariae formula granule characteristic spectrum and establishing method thereof
CN104316613A (en) Method for establishing fingerprint spectrum of wind-dispelling and detoxifying capsules
CN101816715B (en) Method for measuring content of Danshensu in shenshuaining capsules by utilizing HPLC method
CN104007198B (en) A kind of glossy ganoderma emperor's preparation HPLC standard finger-print and construction method thereof and application
CN105510452B (en) Multi-target ingredient assay, fingerprint map construction and the preparation method of liver-benefiting eye-brightening oral liquid
CN103424476A (en) Method for simultaneously determining four water-soluble components in polydanshinolic acid
CN104155399B (en) A kind of method of quality control of four rhizoma cyperi medicine materical crude slice processed
CN103389353A (en) Ultra-high performance liquid chromatography method for determination of content of phenolic acid components in blood-nourishing cephalocathartic particles
CN106841467A (en) The high-efficiency liquid chromatography method for detecting of amarogentin in a kind of female biochemistry mixture of benefit
CN106706835A (en) Quality detection method of trollius chinensis bunge effervescent tablets
CN109709222A (en) A kind of component detection method of cold drug and compound cold drug
CN108226359A (en) The method for measuring component content in ease pill
CN108333289A (en) A kind of method of multi-analyte immunoassay control grub content
CN104678011B (en) A kind of detection method of TONGMAIYANGXINWAN
Ghosh et al. Development and validation of dissolution test method for andrographolide from film coated polyherbal tablet formulation
CN107917978A (en) The detection method of ethylene glycol in a kind of pigment lotion
CN103901147A (en) Method for measuring dissolution rate of andrographolide pills
CN113820411A (en) Method for measuring contents of schizandrol A and schizandrol B in preparation for strengthening body resistance and removing blood stasis
CN103901138B (en) A kind of quality determining method of the supplemental treatment preparation for carcinosis radiotherapy and chemotherapy

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170613

RJ01 Rejection of invention patent application after publication