CN100387243C - Quality control method of ixeris sonchifolia injection - Google Patents
Quality control method of ixeris sonchifolia injection Download PDFInfo
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Abstract
The present invention relates to a quality control method of sowthistle-leaf ixeris seedling injections, which mainly comprises items of characteristic, identification, checking, fingerprint and assay and is characterized in that the present invention takes sowthistle-leaf ixeris seedling contrasting to medicinal materials, total flavonoids, sweet osmanthus grass element glycoside, adenosine, sesquiterpene lactone, total coumarin and triterpenoid saponin as the detecting indexes of the quality control of the Chinese traditional medicine injections. The present invention makes the medicinal materials and finished products have good correlation, and the fingerprint of the sowthistle-leaf ixeris seedling injections researched by the applicant can perfectly control product quality.
Description
(1) technical field
The invention belongs to technical field of Chinese medicine, specifically relate to a kind of method of quality control of KUDIEZI ZHUSHEYE.
(2) background technology
KUDIEZI ZHUSHEYE is the modern Chinese medicine preparation, with the Herba Ixeritis Sonchifoliae is that raw material is made, have promoting blood circulation and stopping pain, heat clearing away blood stasis dispelling, the expansion coronary vasodilator, improve the supply of myocardium blood oxygen, increase the fibrinoclase activity, suppress thrombotic effect, the injection that is used for coronary heart disease, angina pectoris, cerebral thrombosis, cerebral infarction etc. also is used for the treatment of diseases such as fundus oculi disease, malignant tumor, viral pneumonia, viral hepatitis, optic atrophy, diabetic complication, vasculitis, cervical spondylosis at present clinically.KUDIEZI ZHUSHEYE is on the basis that guarantees the constant product quality controllable safety, more new development constantly, in order better to control the quality of said preparation, guarantee the safety of medication, instruct better and produce, make technology controlling and process rationally strict more, make consumer's energy full appreciation product quality, need research, control this injection method for quality.
(3) summary of the invention
The objective of the invention is to: a kind of method of quality control of KUDIEZI ZHUSHEYE is provided, and this method provides means, technical method of the index that detects, detection or the like to relevant production, testing agency; So that control the quality of said preparation better, guarantee the safety of medication, can instruct production better, make controlling of production process rationally strict more, make consumer's energy full appreciation product quality.
The present invention constitutes like this: the method for quality control of KUDIEZI ZHUSHEYE, mainly comprise projects such as character, discriminating, inspection, finger printing, assay, it relates to the Chinese medicine injection made from Herba Ixeritis Sonchifoliae medical material or its extract or contains the method for quality control of the injection that various effective sites use, and this method of quality control is with Herba Ixeritis Sonchifoliae control medicinal material, total flavones, luteolin glycosides, adenosine, sesquiterpene lactones, total coumarins, the triterpene saponin detection index as the quality control of this Chinese medicine injection.
The detection index of above-mentioned quality control index can be preferably: with adenosine, luteolin and glycosides thereof, total flavones, the Herba Ixeritis Sonchifoliae control medicinal material detection index as the discrimination method of this Chinese medicine injection.
The detection index of above-mentioned quality control index can be preferably: with Herba Ixeritis Sonchifoliae control medicinal material, total flavones, luteolin glycosides, adenosine, sesquiterpene lactones, total coumarins, the triterpene saponin detection index as the content assaying method of this Chinese medicine.
The detection index of above-mentioned quality control index can be preferably: with adenosine, luteolin and glycosides thereof, total flavones, Herba Ixeritis Sonchifoliae control medicinal material, the sesquiterpene lactones detection index as the finger printing research of this Chinese medicine.
The character of above-mentioned KUDIEZI ZHUSHEYE is that sundown is to brown xanchromatic clear liquid.
In the method for quality control of a kind of KUDIEZI ZHUSHEYE of the present invention,, can adopt following method for the authentication technique of Herba Ixeritis Sonchifoliae:
1: adopt thin layer chromatography, generally use silica gel G or silica GF254 or silica gel H to be lamellae, the point sample amount is an a certain volume between 0.5～30ul, with the Herba Ixeritis Sonchifoliae control medicinal material, with adenosine product in contrast, sample pre-treatments comprises direct sample, with methods such as reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, isopropyl alcohol, acetone, water, methanol, formic acid, dichloromethane, ethyl acetate, glacial acetic acid, ammonia, at least a certain proportion according to routine in the n-butyl alcohol is formulated, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 2～30% sulphuric acid ethanol, or spray is with the method for solution such as 1～10% 1,2,3-indantrione monohydrate ethanol colour developing.
2: adopt high performance liquid chromatography, sample pre-treatments comprises direct sample, with methods such as reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, the general chromatographic column of using C8 or C18 type filler, is mobile phase with at least a solvent in acetonitrile, water, methanol, the phosphoric acid under the proper ratio condition of routine, with Herba Ixeritis Sonchifoliae control medicinal material, adenosine, luteolin glycosides product in contrast, detect wavelength in 200～500nm scope.
In the method for quality control of a kind of KUDIEZI ZHUSHEYE of the present invention, described inspection: comprise pH value, content uniformity, clarity, aseptic, particulate matter, protein, tannin, resin, CAOSU salt, sulfate, calcium salt, potassium ion, heavy metal, arsenic salt, pesticide residues etc. are project or some projects all, concrete detection method and being consistent that the Chinese Pharmacopoeia appendix of current edition at that time records, potassium ion, heavy metal, the detection method of arsenic salt also comprises with Microwave Digestion handles sample, and then adopts atomic absorption method, plasma emission spectrum or inductively coupled plasma mass spectrum (ICP-MS) method are carried out method for measuring; Specification requirement in the medicine is: (1) pH value is between 2～10; (2) heavy metal must not cross 20/1000000ths: (3) arsenic salt must not cross 2/1000000ths; (4) the residual total amount of organochlorine pesticide must not cross 1,000,000/; (5) the contrast liquor ratio made by inspection of Chinese Pharmacopoeia appendix and standard potassium sulfate solution 1ml of sulfate must not denseer (0.005%); (6) calcium salt is got this product 2ml, adds ammonium oxalate test solution 1ml, shakes up, and places 10 minutes, muddiness must not occur.
In the method for quality control of a kind of KUDIEZI ZHUSHEYE of the present invention: for finger printing, adopt high performance liquid chromatography, sample pre-treatments comprises direct sample, can take:
(1) with methods such as reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, acetonitrile, water, 0.1～10% glacial acetic acid, sodium heptanesulfonate, at least a solvent in dimethylmethane 0.4% phosphoric acid is a mobile phase under the proper ratio condition of routine, method with gradient or isocratic elution is separated, detect wavelength in 200～600nm scope, with adenosine, luteolin and glycosides thereof, total flavones, all or part of kind is as characteristic fingerprint peak or internal standard substance peak in Herba Ixeritis Sonchifoliae control medicinal material and the extract thereof.
(2) using the chromatographic column of C18 type filler, is 0.4% phosphoric acid solution with A, and B is a mobile phase for the second eyeball, separates with the method for gradient elution, and the detection wavelength is 348nm, with luteolin-7-O-β-D-glucuronide as characteristic fingerprint peak or internal standard substance peak.
In the method for quality control of a kind of KUDIEZI ZHUSHEYE of the present invention, adopt following method for assay:
1: with the general flavone content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample, with methods such as reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 400～600nm, general standard curve method or the reference substance method of adopting measured, and reference substance commonly used is rutin, luteolin and glycosides thereof.For the assay also visible total coumarins content in ultraviolet light spectrophotometry this product, sample.
2: with the adenosine in high effective liquid chromatography for measuring this product and luteolin-7-O-β-D-glucuronide content, sample pre-treatments comprises direct sample, with methods such as reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～600nm, generally adopts standard curve method or reference substance method to measure.
3: adopt the luteolin-7-O-β-D-glucuronide in liquid chromatography for measuring this product, sample pre-treatments is direct sample, using the chromatographic column of C18 type filler, is mobile phase with acetonitrile, 0.4% phosphoric acid solution under the proper ratio condition of routine, and the detection wavelength is 48nm.
Compared with prior art, the index components that the present invention chooses is the important effective active composition of product, is very necessary to the control drug quality, and is very desirable as the index of content control.The applicant be in order to pick up product quality from the source, under the prerequisite of fixedly traditional Chinese medicinal materials assortment, the place of production and collection period, formulates the finger printing of Chinese crude drug, effective site or intermediate, injection.
Utilize method of quality control provided by the invention for proof and can control a kind of product quality of KUDIEZI ZHUSHEYE better, the medicine that obtains has effective effect, and the applicant has carried out a series of experiments;
The experimental example 1 different places of production and collection period the medical material measurement result
Batch luteolin-7-O-β-D-glucuronide content (%)
030501 0.131
030502 0.130
030503 0.169
030510 0.085
030511 0.141
030512 0.115
030601 0.213
030602 0.165
030603 0.221
030604 0.152
Above-mentioned result of study shows payes attention to the medical material place of production and collection period, significant for assurance and raising quality of medicinal material, most important for control finished product curative effect.
The research of experimental example 2 finger printing
1, having investigated (1) acetonitrile one water (gradient elution) (2) A in the selection research process of mobile phase respectively is 0.4% phosphoric acid, and B is two kinds of flow phase system of acetonitrile (gradient elution).The result shows under mobile phase (1) condition that the peak hangover is serious, and it is incomplete to go out the peak; Under mobile phase (2) condition, peak shape is better, goes out the peak fully and be evenly distributed, so selected.
2, detect wavelength determination
Investigated the chromatographic peak situation under different-waveband typical wavelengths 300,325,348,356 respectively, the result shows that chromatographic peak is more under 348nm, and peak shape is better, so finally select for use 348nm as detecting wavelength.
3, the foundation of finger printing and analysis
By above-mentioned chromatographic condition, respectively 10 batches of KUDIEZI ZHUSHEYE are measured, investigate the concordance of 10 batch sample liquid chromatograph.From collection of illustrative plates, 9min had 2 small peaks in the past, and was widely different in each batch data of preparation, raw material, and it is very little to account for full spectrum amount, so on chromatographic peak is handled, integration and calculating are not carried out in the zone before the 9min.Investigating the chromatogram of 10 batch samples, find out its metastable total peak, is that other peaks are demarcated in order with Arabic numerals with reference to peak (No. 6 peaks) with the luteolin peak, and KUDIEZI ZHUSHEYE is demarcated 8 peaks altogether.Relative retention time and relative peak area ratio with the reference peak are 1, calculate the relative retention time and the ratio that accounts for the peak area of total peak area more than 5% of each total fingerprint peaks.With the meansigma methods of relative retention time, as the relative retention time of standard finger-print separately, with meansigma methods ± 10% allow mobility scale as relative retention time.
According to the regulation of " Chinese medicine finger printing research specification requirement (provisional) ", in this finger printing, have only No. 1, No. 6, the percentage ratio that No. 7 unimodal areas in peak account for total peak area may surpass 20%, and the percentage ratio that the three accounts for the total peak area sum surpasses 80%.No. 6 peaks are with the meansigma methods of the 10 batch sample relative peak area ratios ratio as standard finger-print, with meansigma methods ± 25% determine its allowed band, be 0.23-0.37.
4, correlation analysis
The peak shape and the global feature good relationship of KUDIEZI ZHUSHEYE and the two finger printing of raw material Herba Ixeritis Sonchifoliae medical material thereof.
5, the similarity analysis of finger printing
The finger printing similarity evaluation software that the utilization pharmacopeia can provide is handled each finger printing and integration data thereof through computed in software, the finger printing of KUDIEZI ZHUSHEYE 10 batch samples all has similarity preferably as a result, and similarity is all greater than 0.9.
6, finger printing and every technical parameter
Relevant parameter according to 10 batches of KUDIEZI ZHUSHEYE HPLC spectrums provide compares the test sample spectrogram, and wherein 8 peaks are that each batch sample is common, determines that therefore these 8 peaks are total fingerprint peaks.In total fingerprint peaks, the peak area that has only No. 1, No. 6 and No. 7 peak is greater than 10% of total peak area, so only consider the peak area ratio at these three peaks, all the other each total peaks are all qualitative by its relative retention time.
KUDIEZI ZHUSHEYE fingerprint pattern technology parameter: the peak number (relative retention time) at total peak:
1(9.719)，2(10.281)，3(10.846)，4(18.368)，5(23.302)，6(24.240)，7(24.413)，8(29.545)。
The result shows that medical material, finishing room have good dependency, and the KUDIEZI ZHUSHEYE finger printing of the applicant's research can the better controlled product quality.
(4) concrete embodiment:
Embodiments of the invention 1: a kind of method of quality control of KUDIEZI ZHUSHEYE mainly comprises character, discriminating, inspection, finger printing, assay project.
1, character: this Chinese medicine injection is that sundown is to brown xanchromatic clear liquid.
2, differentiate: for the discriminating of adenosine: adopt thin layer chromatography, use silica gel G F
254Lamellae, point sample amount are 5ul, and with adenosine product in contrast, direct sample, developing solvent are that chloroform, ethyl acetate, isopropyl alcohol, ammonia, water are formulated according to conventional ratio, and the condition of inspecting is the method for inspecting under the ultraviolet.
3, check: comprise all projects or some projects such as pH value, content uniformity, clarity, aseptic, particulate matter, protein, tannin, resin, oxalates, calcium salt, sulfate, potassium ion, heavy metal, arsenic salt, pesticide residues, concrete detection method and being consistent that the Chinese Pharmacopoeia appendix of current edition at that time records, the detection method of potassium ion, heavy metal, arsenic salt also comprises with Microwave Digestion handles sample, and then adopts atomic absorption method, plasma emission spectrum or inductively coupled plasma mass spectrography to carry out method for measuring; Specification requirement in the medicine is: (1) pH value is between 2～10; (2) heavy metal must not cross 20/1000000ths: (3) arsenic salt must not cross 2/1000000ths; (4) the residual total amount of organochlorine pesticide must not cross 1,000,000/; (5) the contrast liquor ratio made by inspection of Chinese Pharmacopoeia appendix and standard potassium sulfate solution 1ml of sulfate must not denseer (0.005%); (6) calcium salt is got this product 2ml, adds ammonium oxalate test solution 1ml, shakes up, and places 10 minutes, muddiness must not occur.
4, finger printing: adopt high performance liquid chromatography, sample pre-treatments comprises direct sample, use the chromatographic column of C8 or C18 type filler, with acetonitrile, 0.4% phosphoric acid solution is mobile phase under the proper ratio condition, method with gradient elution is separated, detect wavelength in the 348nm scope, with luteolin-7-O-β-D-glucuronide as characteristic fingerprint peak or internal standard substance peak.Finger printing and gradient are as follows:
KUDIEZI ZHUSHEYE finger printing gradient elution table
| Time gradient | Acetonitrile A (%) | 0.4% phosphoric acid solution B (%) |
| 0 minute | 10 | 90 |
| 40 minutes | 31 | 69 |
| 40.01 minute | 10 | 90 |
| 45 minutes | 10 | 90 |
5, assay:
Method 1: with the general flavone content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample: with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, the mensuration wavelength is 505nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is rutin or luteolin-7-O-β-D-glucuronide, and every 10ml contains total flavones must not be less than 4.0mg.
Method 2: for assay: also can measure adenosine content in this product with liquid phase method, sample pre-treatments comprises direct sample, with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with one or more kind solvents in acetonitrile, water, 0.4% phosphoric acid is that mobile phase mensuration wavelength is 260nm under the proper ratio condition of routine, adopt standard curve method or reference substance method to measure, every 10ml contains total flavones must not be less than 0.025mg.
Method 3: with the luteolin in high effective liquid chromatography for measuring this product-7-O-β-D-glucuronide.Sample pre-treatments comprises direct sample, with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, is mobile phase with one or more kind solvents in acetonitrile, 0.4% phosphoric acid under the proper ratio condition of routine, with luteolin glycosides product in contrast, detect wavelength in the 348nm scope, every 10ml contains luteolin-7-O-β-D-glucuronide must not be less than 0.60mg.
Claims (5)
1. the method for quality control of a KUDIEZI ZHUSHEYE, mainly comprise character, discriminating, inspection, finger printing, assay project, it is characterized in that: it is with Herba Ixeritis Sonchifoliae control medicinal material, total flavones, luteolin glycosides, adenosine, sesquiterpene lactones, total coumarins, the triterpene saponin detection index as the quality control of this Chinese medicine injection; The character of this Chinese medicine injection is that sundown is to brown xanchromatic clear liquid;
Described discrimination method adopts thin layer chromatography, generally use silica gel G or silica GF254 or silica gel H to be lamellae, the point sample amount is an a certain volume between 0.5～30ul, with the Herba Ixeritis Sonchifoliae control medicinal material, adenosine is product in contrast, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent is chloroform or acetone, formic acid, water, methanol, dichloromethane, ethyl acetate, glacial acetic acid, at least a formulated in the n-butyl alcohol according to conventional certain proportion, the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 2～30% sulphuric acid ethanol, or spray is with the method for 1～10% ethanol solution of ninhydrin colour developing;
Described inspection comprises pH value, content uniformity, clarity, aseptic, particulate matter, protein, tannin, resin, oxalates, potassium ion, heavy metal, arsenic salt, pesticide residues, calcium salt, the whole projects of sulfate or some projects, what the Chinese Pharmacopoeia appendix of concrete detection method and current edition recorded is consistent, the detection method of potassium ion, heavy metal, arsenic salt also comprises with Microwave Digestion handles sample, and then adopts atomic absorption method, plasma emission spectrum or inductively coupled plasma mass spectrography to carry out method for measuring; Specification requirement in the KUDIEZI ZHUSHEYE is: (1) pH value is between 2～10, and (2) heavy metal is no more than 20/1000000ths, and (3) arsenic salt is no more than 2/1000000ths, and the residual total amount of (4) organochlorine pesticide is no more than 1,000,000/;
Described finger printing: adopt high performance liquid chromatography, sample pre-treatments comprises direct sample: with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, acetonitrile, water, 0.1～10% glacial acetic acid, sodium heptanesulfonate, dimethylmethane, at least a solvent in 0.4% phosphoric acid is a mobile phase under the proper ratio condition of routine, method with gradient or isocratic elution is separated, detect wavelength in 200～600nm scope, with total flavones, the luteolin glycosides, adenosine, sesquiterpene lactones, total coumarins, all or part of composition is as characteristic fingerprint peak or internal standard substance peak in the triterpene saponin;
Described assay is with the general flavone content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate, chloroform, dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 400～600nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is rutin, luteolin glycosides; For assay with the total coumarins content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample, with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 400～600nm, adopts standard curve method or reference substance method to measure.
2. according to the method for quality control of the described KUDIEZI ZHUSHEYE of claim 1, it is characterized in that: for the discrimination method of Herba Ixeritis Sonchifoliae: adopt high performance liquid chromatography, sample pre-treatments comprises direct sample, method with reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, methanol, at least a kind solvent in the phosphoric acid is a mobile phase under the proper ratio condition of routine, with the Herba Ixeritis Sonchifoliae control medicinal material, adenosine, the luteolin glycosides is product in contrast, detect wavelength in 200～500nm scope.
3. according to the method for quality control of the described KUDIEZI ZHUSHEYE of claim 1, it is characterized in that: for the discriminating of adenosine: adopt thin layer chromatography, use silica gel G F
254Lamellae, point sample amount are 5ul, and with adenosine product in contrast, direct sample, developing solvent are that chloroform, ethyl acetate, isopropyl alcohol, ammonia, water are formulated according to conventional ratio, and the condition of inspecting is the method for inspecting under the ultraviolet.
4. according to the method for quality control of the described KUDIEZI ZHUSHEYE of claim 1, it is characterized in that: adopt liquid chromatography for finger printing, sample pre-treatments is direct sample, use the chromatographic column of C18 type filler, with 0.4% phosphoric acid solution, or the second eyeball is mobile phase, separates with the method for gradient elution, the detection wavelength is 348nm, with luteolin-7-O-β-D-glucuronide as characteristic fingerprint peak or internal standard substance peak.
5. according to the method for quality control of the described KUDIEZI ZHUSHEYE of claim 1, it is characterized in that: adenosine, luteolin glycosides, total flavones, Herba Ixeritis Sonchifoliae control medicinal material detection index as discrimination method, content assaying method and the finger printing research of this Chinese medicine injection.
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| CN103115985B (en) * | 2013-03-07 | 2014-04-02 | 通化华夏药业有限责任公司 | Method for synchronously detecting six flavonoid constituents in sowthistle-leaf ixeris seedling injection in HPLC-DAD (High Performance Liquid Chromatography-Diode Array detector) method |
| CN106501440B (en) * | 2016-10-24 | 2018-01-05 | 中悦民安（北京）科技发展有限公司 | The discrimination method of field pennycress in Chinese medicine compound prescription |
| CN106841434A (en) * | 2017-01-17 | 2017-06-13 | 华楠 | Ixeris Sonchifolia Hance injection fingerprint checking method |
| CN113473863B (en) | 2019-02-03 | 2023-10-03 | 特尔维瓦股份有限公司 | Method for controlling black leaf spot in bananas using water yellow oil and its formulation |
| CN110297061B (en) * | 2019-07-25 | 2021-09-21 | 广西中医药大学 | Method for determining contents of chlorogenic acid, caffeic acid and luteolin in Ixeris denticulata by one-test-multiple-evaluation method |
| CN110297060B (en) * | 2019-07-25 | 2021-09-17 | 广西中医药大学 | Fingerprint detection method and fingerprint thereof for ixeris sonchifolia medicinal materials |
| CN110907526A (en) * | 2019-11-27 | 2020-03-24 | 亚宝药业集团股份有限公司 | Test method for rapidly and quantitatively detecting potassium ions in safflower injection |
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| CN1346648A (en) * | 2001-06-24 | 2002-05-01 | 吉林省通化白山药业股份有限公司 | Diemailing injection and its preparing process |
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