CN104502502A - QAMS for detecting content of organic acids in sowthistle-leaf ixeris seedling injection - Google Patents
QAMS for detecting content of organic acids in sowthistle-leaf ixeris seedling injection Download PDFInfo
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Abstract
The invention relates to the field of analysis of traditional Chinese medicine components, and relates to QAMS for detecting the content of organic acids in sowthistle-leaf ixeris seedling injection. The QAMS disclosed by the invention comprises the following steps: (1), setting chromatographic conditions; (2), preparing a reference solution; (3), preparing a test solution; and (4), calculating correction factors. Relative correction factors of chicoric acid, mono-caffeoyl tartaric acid, chlorogenic acid and caffeic acid are calculated by taking chicoric acid as the internal reference compound, and used as constants for detecting the content; correction factors are calculated by taking effective active components in the sowthistle-leaf ixeris seedling injection and high-content chicoric acid as internal reference compounds; the content of mono-caffeoyl tartaric acid, chlorogenic acid and caffeic acid in the sowthistle-leaf ixeris seedling injection are calculated; the content of the four organic acids in the injection can be detected simultaneously; therefore, the quality of the sowthistle-leaf ixeris seedling injection in industrial production can be monitored scientifically, sensitively and rapidly; and simultaneously, the problem that the quality of the sowthistle-leaf ixeris seedling injection cannot be controlled objectively and reasonably because of shortage of reference substances can be solved.
Description
technical field
The present invention relates to traditional Chinese medicine ingredients analysis field, namely a survey comments method to measure organic acid content in Ixeris Sonchifolia Hance injection more.
Background technology
In the prior art, sowthistle-leaf ixeris seedling another name babysbreath, denticulate ixeris herb, mainly be distributed in the ground such as China northeast and the Inner Mongol, for the raw then dry herb of feverfew irexis sonchifolia (Ixeris sonchifolia (Bge.) Hance), cold in nature, bitter, pungent, there is effect that is clearing heat and detoxicating, apocenosis pain relieving
[1].Sowthistle-leaf ixeris seedling (Die mai ling) parenteral solution take sowthistle-leaf ixeris seedling as the intravenous fluid of raw material Hydrolysis kinetics, has promoting blood circulation and removing blood stasis, improve microcirculatory effect
[2].This parenteral solution has gone on the market for many years, determined curative effect.Experimental study shows, Ixeris Sonchifolia Hance injection chemical composition more complicated, and the main active relevant to its clinical efficacy is organic acid, flavonoids and gradient elution.
Ixeris Sonchifolia Hance injection (former name: Diemailing injection) lists national drug standards product (the accurate word Z20025450 of traditional Chinese medicines) in, is produced by Tonghua Huaxia Pharmaceutical Co., Ltd..
Prescription: irexis sonchifolia 1000g, makes 1000ml.
Method for making: get irexis sonchifolia, boiling secondary, 1 hour first time, second time 0.5 hour, collecting decoction, be concentrated into every 1ml and be equivalent to crude drug in whole 0.5g, let cool to less than 40 DEG C, under agitation add 10% calcium oxide breast adjust ph to 10, place 12 hours, centrifugal, centrifugal sediment is weighed, be suspended in 5.3 times amount 95% ethanol (making alcohol content reach 80%), add 50% sulfuric acid solution adjust ph to 3-4, abundant stirring makes to react completely, centrifugal, centrifugate adds in 40% sodium hydroxide solution and pH value to 7.0, filter, filtrate recycling ethanol, and wave most ethanol, be diluted to every 1ml with water for injection and be equivalent to crude drug in whole 4g, put less than-5 DEG C to place more than 12 hours, filter, filtrate adds 0.1-0.2% medical active carbon powder, boil 15 minutes, put less than-5 DEG C to place more than 24 hours, filter, filtrate injecting is diluted with water to ormal weight, adjust ph is to 7.0-7.5, filter, embedding, sterilizing, obtain.Proterties: this product is the clear liquid of light yellowish brown to yellowish-brown.
Assay: assay: the every 10ml of this product contains general flavone with anhydrous rutin (C
27h
30o
16) meter, must not 4.0mg be less than.Containing irexis sonchifolia with adenosine (C
10h
12n
5o
4) meter, must not 0.025mg be less than.
Function cures mainly: promoting blood circulation and stopping pain, Qingre Quyu.For the obstruction of qi in the chest of hemostasis impatency, card is shown in: uncomfortable in chest, pained, bitter taste, and tongue is dark red or deposit ecchymosis etc.Be applicable to coronary heart diseases and angina pectoris and see above-mentioned symptom person.Also the person that can be used for cerebral infarction.
Usage and dosage: drip-feed, a 10-40ml, 1 time on the one; Apply after being diluted to 250-500ml with 5% glucose or 0.9% sodium chloride injection; It within 14 days, is a course for the treatment of; Or follow the doctor's advice.
Specification: often prop up dress (1) 10ml, (2) 20ml, (3) 40ml.
Experimental study shows, Ixeris Sonchifolia Hance injection chemical composition more complicated, and the main active relevant to its clinical efficacy is organic acid, flavonoids and gradient elution.
About organic acid content testing in Ixeris Sonchifolia Hance injection, Chinese invention patent application book discloses a kind of name and is called " method of five kinds of organic acid component contents in HPLC-DAD method Simultaneously test Ixeris Sonchifolia Hance injection; number of patent application: 201310071078.8 ", the specifically method of five kinds of organic acid component contents in HPLC-DAD method Simultaneously test Ixeris Sonchifolia Hance injection, its step is as follows: the preparation of (1) mixing reference substance solution.(2) preparation of need testing solution.(3) determination method: HPLC-DAD method.Chromatographic condition: chromatographic column: Diamonsil C
18(2); Column temperature: 40 DEG C; Determined wavelength: 325 nm; Flow velocity: 1 mLmin
-1; Sample size: 10 μ L; Mobile phase: acetonitrile, 0.1% formic acid water; Condition of gradient elution: 0-15 min, 9% acetonitrile is linearly increased to 11%, 15-16 min is linearly increased to 18% acetonitrile, 16-30 min is linearly increased to 20% acetonitrile, and 30-40 min is linearly increased to 49% acetonitrile, needs five kinds of organic acid reference substances when its shortcoming is and measures, part reference substance price is higher, and the method round of visits is long, measurement operation is complicated, is difficult to the requirement meeting product quality and production run Quality Control high flux sample mensuration.
Summary of the invention
The object of the invention is to provide a kind of one to survey for above-mentioned deficiency comments method to measure organic acid content in Ixeris Sonchifolia Hance injection more.Effective active composition in Ixeris Sonchifolia Hance injection and the higher Cichoric acid of content are as internal standard compound; calculate correction factor; coffee acyl group tartaric acid single in diezi injection liquid, chlorogenic acid, caffeic acid component content are calculated; can the content of 4 kinds of Determination of Organic Acids in Simultaneously test parenteral solution; can realize science, sensitive, the quality of monitoring Ixeris Sonchifolia Hance injection in commercial production rapidly, can solve cannot the objective problem reasonably controlling Ixeris Sonchifolia Hance injection quality because reference substance lacks simultaneously.
Technical solution of the present invention is: a survey comments method to measure organic acid content in Ixeris Sonchifolia Hance injection more, it is characterized in that step is as follows:
(1) chromatographic condition:
Chromatographic column: Diamonsil C18, Symmetry C18.
Column temperature: 35 DEG C; Determined wavelength: 330nm.
Flow velocity: 1.0 ml/min.
Sample size: 10 μ L.
Mobile phase: A is 0.4% phosphoric acid-H
2o, B are acetonitrile, by carrying out gradient elution below.
Time 0.1min, A phase 98%, B phase 2%; Time 5min, A phase 96%, B phase 4%; Time 10min, A phase 90%, B phase 10%; Time 36min, A phase 75%, B phase 25%; Time 40min, A phase 50%, B phase 50%.
(2) preparation of reference substance solution: precision takes single coffee acyl group tartaric acid standard items 4.00 mg, caffeic acid standard items 1.00 mg, chlorogenic acid standard items 1.20 mg, forulic acid standard items 0.400mg, Cichoric acid standard items 4.00mg, put respectively in measuring bottle, first add 50% methyl alcohol and dissolve constant volume again, shake up, obtain reference substance stock solution; Draw each reference substance stock solution, make containing single coffee acyl group tartaric acid 120.0 μ gmL
-1, caffeic acid 20.00 μ gmL
-1, chlorogenic acid 24 .00 μ gmL
-1, forulic acid 8.000 μ gmL
-1, Cichoric acid 120.0 μ gmL
-1mixing reference substance solution.
(3) preparation of need testing solution: get Ixeris Sonchifolia Hance injection, open after shaking up, 50% methanol dilution is parenteral solution volume 2 times, crude drug 0.5gmL
-1, 0.45 μm of filter membrane filters, and obtains need testing solution.
(4) correction factor calculates, and take Cichoric acid as internal reference thing, calculates Cichoric acid and single coffee acyl group tartaric acid, chlorogenic acid, caffeinic relative correction factor, it can be used as constant for assay.
Advantage of the present invention is: 1, utilize Effective Component of Chinese Medicine intrinsic function relation and proportionate relationship; take Cichoric acid as internal reference thing; calculate Cichoric acid and single coffee acyl group tartaric acid, chlorogenic acid, caffeinic relative correction factor; be respectively 1.295,1.410,0.8421, it can be used as constant for assay.And investigated different column temperature, different in flow rate, different chromatographic column, different instrument to the impact of coffee acyl group tartaric acid single in Ixeris Sonchifolia Hance injection, chlorogenic acid, caffeic acid, relative correction factor.Realized the Simultaneously test of multiple composition (other 3 organic acids) by the composition (Cichoric acid) only measured in Ixeris Sonchifolia Hance injection, can be applicable to measure the multiple organic acid composition in Ixeris Sonchifolia Hance injection.2, test shows that adopting relative retention value method to carry out chromatographic peak to the composition to be measured of organic acid in Ixeris Sonchifolia Hance injection locates simple and feasible.The method achieve easy, quick, reliable results, science, specification, one survey the Quality Control target commented more, ensure that Ixeris Sonchifolia Hance injection quality.There is method advanced person, stability and favorable reproducibility, the advantage such as workable, to Mass Control with ensure that curative effect is significant.
Below in conjunction with embodiment, embodiments of the present invention are described in further detail.
Accompanying drawing explanation
Fig. 1 tetra-kinds of organic acid high-efficient liquid phase chromatograms.
Embodiment
Experimental example 1
One survey comments method to measure organic acid content in Ixeris Sonchifolia Hance injection more:
1 experiment material
1.1 instrument
Shimadzu LC-20AT high performance liquid chromatograph (LC-20AT high-pressure pump; SPD-M20A detecting device; SIL-20A injector, the auspicious MODEL320 column oven of additional spectrum).Agilent 1200 high performance liquid chromatograph (1200 degassers; 1200 high-pressure pumps; 1260 detecting devices; 1260 column ovens).Satorius BT 125D type 100,000/electronic analytical balance (Beijing Sai Duolisi company).KH 2200B type ultrasonic cleaner (Kunshan He Chuan ultrasonic instrument company limited).
1.2 reagent
Single coffee acyl group tartaric acid standard items (Tianjin one side Science and Technology Ltd., lot number: AB142C, content >=98%);
Caffeic acid standard items (EYSIN company, lot number: ES-10112201, content >=98%);
Chlorogenic acid standard items (EYSIN company, lot number: ES-11042802 content >=99.0%);
Forulic acid standard items (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110773-201012, content 99.6%);
Cichoric acid standard items (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111752-200902, content 99.9%);
Methyl alcohol (chromatographically pure, Concord Science and Technology Ltd.); Phosphoric acid (analyzing pure, Tianjin chemical reagent wholesaling firm); Acetonitrile (chromatographically pure, Sigma company); Water is ultrapure water (Hangzhou Wahaha Group Co., Ltd).
Ixeris Sonchifolia Hance injection (Tonghua Huaxia Pharmaceutical Co., Ltd., lot number: 130519,130520,130521,130522,130523,130524,130525,130601,130602,130603,130604,130605,130606,130607,130608,130609,130610,130611,130612,130613.
2 methods and result
2.1 chromatographic condition
Chromatographic column: Diamonsil C18 (2) (5 μm, 200 × 4.6 mm) (Di Ma Science and Technology Ltd.)
Symmetry C18 (5 μm, 150 × 3.9mm) (Waters Science and Technology Ltd.)
Column temperature: 35 DEG C; Determined wavelength: 330nm;
Flow velocity: 1.0 ml/min;
Sample size: 10 μ L;
Mobile phase: A is 0.4% phosphoric acid-H
2o, B are acetonitrile, carry out gradient elution by " table 1 ".
Table 1 mobile phase gradient
Each chromatographic peak is separated better with this understanding, and chromatogram is shown in Fig. 1: A. mixing reference substance; B. Ixeris Sonchifolia Hance injection; 1. single coffee acyl group tartaric acid; 2 chlorogenic acids; 3 caffeic acids; 4 Cichoric acids.
The preparation of 2.2 reference substance solution
Precision takes single coffee acyl group tartaric acid standard items 4.00 mg, caffeic acid standard items 1.00 mg, chlorogenic acid standard items 1.20 mg, forulic acid standard items 0.400mg, Cichoric acid standard items 4.00mg; put respectively in measuring bottle; first add a small amount of 50% methyl alcohol and dissolve constant volume again; shake up, obtain reference substance stock solution.Draw each reference substance stock solution appropriate, make containing single coffee acyl group tartaric acid 120.0 μ gmL
-1, caffeic acid 20.00 μ gmL
-1, chlorogenic acid 24 .00 μ gmL
-1, forulic acid 8.000 μ gmL
-1, Cichoric acid 120.0 μ gmL
-1mixing reference substance solution 1#.
The preparation of 2.3 need testing solutions
Get Ixeris Sonchifolia Hance injection, open after shaking up, 50% methanol dilution is parenteral solution volume 2 times of (crude drug 0.5gmL
-1), 0.45 μm of filter membrane filters, and obtains need testing solution.
2.4 methodological study
2.4.1 linear relationship is investigated
Precision measures mixing reference substance solution 1#, gets 5ml and puts in 10 mL measuring bottles and add 50% methanol dilution to scale and shake up, stepwise dilution, obtain 7 variable concentrations series standard solution.Get series standard solution each sample introduction 10 μ L, analyze and record peak area.With reference substance mass concentration C (μ gmL
-1) be horizontal ordinate, peak area (A) is ordinate, tries to achieve regression equation, the results are shown in Table 2 with least square method.
Single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid, Cichoric acid are respectively at 1.875 ~ 120.0 μ gmL
-1, 0.3750 ~ 20.00 μ gmL
-1, 0.3125 ~ 20.00 μ gmL
-1, 0.1250 ~ 8.000 μ gmL
-1, 1.875 ~ 120.0 μ gmL
-1interior linear relationship is good.
The investigation of table 2 linear relationship
2.4.2 precision test
The accurate mixing reference substance solution 10 μ L drawing concentration under " 2.4.1 " item, repeat sample introduction and measure 6 times, METHOD FOR CONTINUOUS DETERMINATION 3 days, record calculated by peak area precision and relative standard deviation (RSD), test findings is in table 3, table 4.
Result shows, single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid, Cichoric acid withinday precision, day to day precision RSD<5%, show that instrument precision is good.
Table 3 withinday precision is investigated
Table 4 day to day precision is investigated
2.4.3 stability test
Get for examination Ixeris Sonchifolia Hance injection (lot number: 130612), room temperature is placed, and makes need testing solution, in 0,2,4,8,12,24h sample introduction analytic record peak area, the results are shown in Table 5.
Result shows, single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, Cichoric acid be peak area RSD < 5% in 24h, and stability is better.Forulic acid peak area RSD in 12 hours is 4.2%, better stable.
Table 5 study on the stability
2.4.4 replica test
With a collection of confession Ixeris Sonchifolia Hance injection, (lot number: 130612) sample, makes need testing solution, parallel preparation 6 parts, analyzes respectively, calculate each constituent concentration and relative standard deviation, the results are shown in Table 6 by chromatographic condition sample introduction under " 2.1 " item in accurate absorption.
Result shows, single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid, Cichoric acid repeatability RSD<5%, shows that instrument repeatability is good.
Table 6 repeatability is investigated
2.4.5 application of sample recovery test
(lot number: 130612), puts in 10ml measuring bottle the need testing solution of accurate absorption known content, respectively the accurate reference substance solution adding certain mass concentration, wherein single coffee acyl group tartaric acid 250.0 μ gmL
-1chlorogenic acid 12.00 μ gmL
-1, caffeic acid 200.0 μ gmL
-1, forulic acid 4.000 μ gmL
-1, Cichoric acid 450.0 μ gmL
-1add 50% methanol dilution to scale; shake up; parallel preparation 6 parts; calculate single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid, Cichoric acid average recovery; the results are shown in Table 7; the average recovery RSD<5% of single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid Cichoric acid, meets methodology requirement.
Table 7 average recovery is investigated
2.5 relative correction factor
2.5.1 relative correction factor measures
Utilize in certain range of linearity; the amount (quality or concentration) of composition is directly proportional to detector response; i.e. W=f (A); be that internal reference thing calculates single coffee acyl group tartaric acid, chlorogenic acid, caffeinic relative correction factor (relative correction factor with Cichoric acid; RCF
f sa,
f sb f sc,
f si), get 7 mixing reference substance solution under " 2.4.1 " item in test, each sample feeding 2 times, measures the peak area of each composition.According to
fcomputing formula:
A in formula
sfor internal reference thing reference substance s peak area, C
sfor internal reference thing reference substance s concentration, A
ifor certain composition reference substance i peak area to be measured; C
ifor certain composition reference substance i concentration to be measured.Test to obtain single coffee acyl group tartaric acid, chlorogenic acid, forulic acid, caffeinic
fbe followed successively by 1.295,1.410,0.8421,0.4624, the results are shown in Table 8.
Each composition relative correction factor in table 8 Ixeris Sonchifolia Hance injection
2.5.2 durability and system suitability evaluation
1. temperature pair
fimpact
Adopt Shimadzu LC-20AT highly effective liquid phase chromatographic system and Diamonsil C18 chromatographic column; investigate different column temperature (34 DEG C respectively; 35 DEG C; 36 DEG C) impact on coffee acyl group tartaric acid single in Ixeris Sonchifolia Hance injection, chlorogenic acid, caffeic acid, forulic acid relative correction factor; the relative correction factor RSD < 5% of result list coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid and internal reference thing Cichoric acid, shows that column temperature is to each composition
fdo not make significant difference, the results are shown in Table 9.
The different column temperature of table 9 is on the impact-Shimadzu LC-20AT (n=2) of correction factor
2. flow velocity pair
fimpact
Adopt Shimadzu LC-20AT highly effective liquid phase chromatographic system and Diamonsil C18 chromatographic column; investigate mobile phase different in flow rate (0.9ml/min respectively; 1.0ml/min; 1.1ml/min) on the impact of coffee acyl group tartaric acid single in Ixeris Sonchifolia Hance injection, chlorogenic acid, caffeic acid, forulic acid relative correction factor; the relative correction factor RSD < 5% of result list coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid and internal reference thing Cichoric acid, shows that flow velocity is to each composition
fdo not make significant difference, the results are shown in Table 10.
Table 10 different in flow rate is on the impact-Shimadzu LC-20AT (n=2) of correction factor
Comprehensive different column temperature, different in flow rate, different chromatographic column are on the impact of coffee acyl group tartaric acid single in Ixeris Sonchifolia Hance injection, chlorogenic acid, caffeic acid, forulic acid relative correction factor; the RSD that affects of the relative correction factor of single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid, forulic acid and internal reference Cichoric acid is followed successively by 0.9%, 1.2%, 1.9%, 1.4%, shows that column temperature, Flow Chromatography post are to each composition
fdo not make significant difference, the results are shown in Table 11.
Table 11 Different factor is on the impact-Shimadzu LC-20AT (n=2) of correction factor
3. different instrument pair
fimpact
Adopt Shimadzu LC-20AT highly effective liquid phase chromatographic system and Agilent1200 highly effective liquid phase chromatographic system; investigate the impact of different instrument on coffee acyl group tartaric acid single in Ixeris Sonchifolia Hance injection, chlorogenic acid, caffeic acid, forulic acid relative correction factor; the correction factor RSD < 5% of result list coffee acyl group tartaric acid and internal reference thing Cichoric acid; the correction factor RSD > 5% of chlorogenic acid, caffeic acid, forulic acid and internal reference thing Cichoric acid; show that relative correction factor repeatability is poor on different instrument, the results are shown in Table 12.
The different instrument of table 12 and chromatographic column record each composition relative correction factor
2.6 component chromatographic peak location to be measured
Apply Shimadzu LC-20AT highly effective liquid phase chromatographic system and Agilent1200 highly effective liquid phase chromatographic system in test to have investigated respectively and adopt retention time difference and the reappearance of relative retention value in different brands chromatographic column, it is less that result shows to adopt relative retention value fluctuation, therefore adopts relative retention value method to carry out chromatographic peak to the composition to be measured of organic acid in Ixeris Sonchifolia Hance injection and locate comparatively feasible.Relative retention value refers to the ratio of retention time between each composition to be measured and internal reference thing s, computing formula:
r as=
t ra/
t rs.(t
racomposition retention time to be measured, t
rsinternal reference thing retention time).
The relative retention value RSD < 5% of result list coffee acyl group tartaric acid, chlorogenic acid, forulic acid, caffeic acid and internal reference thing Cichoric acid, utilizes relative retention value feasible to chromatographic peak location, the results are shown in Table 13 under showing this chromatographic condition.
The location relative retention value method of table 13 QAMS method composition chromatographic peak to be measured
Method and external standard method results contrast are commented in 2.7 1 surveys more
Get 20 batches of Ixeris Sonchifolia Hance injection (lot numbers: 130519, 130520, 130521, 130522, 130523, 130524, 130525, 130601, 130602, 130603, 130604, 130605, 130606, 130607, 130608, 130609, 130610, 130611, 130612, 130613) appropriate, test solution is prepared by under " 2.3 " item, sample introduction is analyzed, record peak area, adopt external standard method and to survey and comment method (quantitative analysis of multi-components by single marker more, QAMS method) calculate Cichoric acid, single coffee acyl group tartaric acid, chlorogenic acid, (survey comments method to be applicable to have the mensuration of high level composition to caffeic acid content more, in test, ferulaic acid content is lower, external standard method institute's measured value and QAMS method institute measured value deviation > 5%, unlisted temporarily at this).
The results are shown in Table 14; display employing two kinds of method gained content are without significant difference; single coffee acyl group tartaric acid, chlorogenic acid, caffeic acid relative deviation [RD=(external standard measured value-QAMS method calculated value)/external standard method measured value] are respectively 1.137%, 3.611%, 2.966%; equal < 5%, shows that QAMS method can be used for the mensuration of these 4 kinds of compositions.
Table 14 one is surveyed and is commented method and external standard method results contrast more
3 brief summaries
3.1 1 survey the location of commenting method chromatographic peak to be measured more
One surveys and comments method implication to be more: utilize the amount of composition in range of liner (quality or concentration) to be directly proportional to detector response, realizes multiple composition (seldom, high, the unstable person of preparation cost) Simultaneous Determination by measuring a composition (reference substance is easy to get, inexpensive, responder).Not only solve Chinese medicine multicomponent quantitatively and the reference substance existed in multi objective quality control lack problem, realize multi objective synchronizing quality simultaneously and control to reflect traditional Chinese medicine quality.
The accurate location of composition chromatographic peak to be measured is the prerequisite guaranteeing that a survey is commented method (QAMS) more and applied, the general chromatographic peak adopting retention time difference or relative retention time to locate composition to be measured.Test shows that adopting relative retention value method to carry out chromatographic peak to the composition to be measured of organic acid in Ixeris Sonchifolia Hance injection locates comparatively feasible.
3.2 relative correction factor reappearances
For making QAMS method have good applicability, investigated respectively different column temperature, different in flow rate and different size, model chromatographic column on the impact of RCF, result shows, RCF has good reappearance.The content value that QAMS method and external standard method obtain is basically identical, show that QAMS method more accurately can carry out quantitative measurement to organic acid compositions such as single coffee acyl group tartaric acids in Ixeris Sonchifolia Hance injection, but between different instrument, RCF has different, needs to be investigated further.
Establish a survey comments method to measure the analytical approach of organic acid composition in Ixeris Sonchifolia Hance injection more, survey to employing external standard method and an organic acid content commenting method to record to compare more simultaneously, the content value that QAMS method and external standard method obtain is basically identical, shows that a survey comments method to can be used for the mensuration of organic acid component content in Ixeris Sonchifolia Hance injection more.
Claims (1)
1. a survey comments method to measure organic acid content in Ixeris Sonchifolia Hance injection more, it is characterized in that step is as follows:
(1) chromatographic condition:
Chromatographic column: Diamonsil C18, Symmetry C18;
Column temperature: 35 DEG C; Determined wavelength: 330nm;
Flow velocity: 1.0 ml/min;
Sample size: 10 μ L;
Mobile phase: A is 0.4% phosphoric acid-H
2o, B are acetonitrile, by carrying out gradient elution below:
Time 0.1min, A phase 98%, B phase 2%; Time 5min, A phase 96%, B phase 4%; Time 10min, A phase 90%, B phase 10%; Time 36min, A phase 75%, B phase 25%; Time 40min, A phase 50%, B phase 50%;
(2) preparation of reference substance solution: precision takes single coffee acyl group tartaric acid standard items 4.00 mg, caffeic acid standard items 1.00 mg, chlorogenic acid standard items 1.20 mg, forulic acid standard items 0.400mg, Cichoric acid standard items 4.00mg, put respectively in measuring bottle, first add 50% methyl alcohol and dissolve constant volume again, shake up, obtain reference substance stock solution; Draw each reference substance stock solution, make containing single coffee acyl group tartaric acid 120.0 μ gmL
-1, caffeic acid 20.00 μ gmL
-1, chlorogenic acid 24 .00 μ gmL
-1, forulic acid 8.000 μ gmL
-1, Cichoric acid 120.0 μ gmL
-1mixing reference substance solution;
(3) preparation of need testing solution: get Ixeris Sonchifolia Hance injection, open after shaking up, 50% methanol dilution is parenteral solution volume 2 times, crude drug 0.5gmL
-1, 0.45 μm of filter membrane filters, and obtains need testing solution;
(4) correction factor calculates: take Cichoric acid as internal reference thing, calculates Cichoric acid and single coffee acyl group tartaric acid, chlorogenic acid, caffeinic relative correction factor, it can be used as constant for assay.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950289A (en) * | 2016-01-07 | 2017-07-14 | 陕西步长制药有限公司 | A kind of coronary disease treatment capsule one is surveyed comments detection method of content more |
| CN112903877A (en) * | 2021-03-16 | 2021-06-04 | 吉林农业大学 | Method for simultaneously determining contents of chlorogenic acid, caffeic acid, ferulic acid and chicoric acid in chicory |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102523862A (en) * | 2011-11-16 | 2012-07-04 | 沈阳双鼎制药有限公司 | Cultivation and quality control method for ixeris sonchifolia hance for Kudiezi injection |
| CN103163243A (en) * | 2013-03-07 | 2013-06-19 | 通化华夏药业有限责任公司 | Method for simultaneously determining five organic acid components content in Ixeris sonchifolia Hance injection by HPLC-DAD method |
-
2014
- 2014-12-27 CN CN201410824718.2A patent/CN104502502A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102523862A (en) * | 2011-11-16 | 2012-07-04 | 沈阳双鼎制药有限公司 | Cultivation and quality control method for ixeris sonchifolia hance for Kudiezi injection |
| CN103163243A (en) * | 2013-03-07 | 2013-06-19 | 通化华夏药业有限责任公司 | Method for simultaneously determining five organic acid components content in Ixeris sonchifolia Hance injection by HPLC-DAD method |
Non-Patent Citations (2)
| Title |
|---|
| RAN YIN等: "Determination of five components in Ixeris sonchifolia by high performance liquid chromatography", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 张坤等: "高效液相色谱校正因子法测定苦碟子提取物中5 种主要成分的含量", 《中南药学》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950289A (en) * | 2016-01-07 | 2017-07-14 | 陕西步长制药有限公司 | A kind of coronary disease treatment capsule one is surveyed comments detection method of content more |
| CN106950289B (en) * | 2016-01-07 | 2019-10-29 | 陕西步长制药有限公司 | A kind of coronary disease treatment capsule one is surveyed comments detection method of content more |
| CN112903877A (en) * | 2021-03-16 | 2021-06-04 | 吉林农业大学 | Method for simultaneously determining contents of chlorogenic acid, caffeic acid, ferulic acid and chicoric acid in chicory |
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