CN105372369A - Danhong injection fingerprint determination method - Google Patents
Danhong injection fingerprint determination method Download PDFInfo
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- CN105372369A CN105372369A CN201510773610.XA CN201510773610A CN105372369A CN 105372369 A CN105372369 A CN 105372369A CN 201510773610 A CN201510773610 A CN 201510773610A CN 105372369 A CN105372369 A CN 105372369A
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Abstract
The invention relates to a Danhong injection quality control method, concretely relates to a Danhong injection fingerprint determination method and belongs to the technical field of pharmaceutical analysis. The determination method comprises 1, contrast solution preparation, 2, internal standard solution preparation, 3, sample solution preparation, and 4, high performance liquid chromatography-mass spectrometry analysis determination. An internal standard peak is creatively and quantificationally introduced into a complex fingerprint so that the built method is accurate and simple and has high sensitivity and repeatability. The method realizes comprehensive monitoring of raw material drug, semi-finished product and finished product quality and monitoring of production process stability.
Description
Technical field
The present invention relates to a kind of method of quality control of DANHONG ZHUSHEYE, be specifically related to a kind of finger print measuring method of DANHONG ZHUSHEYE, belong to Pharmaceutical Analysis technical field.
Background technology
DANHONG ZHUSHEYE system, by the drug matching such as the red sage root, safflower, extracts and the compound injection made through processing.DANHONG ZHUSHEYE has effect that is promoting blood circulation and removing blood stasis, that remove obstruction in channels to relieve pain; clinically be usually used in diseases of cardiovascular and cerebrovascular systems; drug efficacy study shows that DANHONG ZHUSHEYE has obvious function of resisting myocardial ischemia; coronary flow can be increased and reduce myocardial consumption of oxygen; there is obvious Cerebral ischemia protection effect; from platelet aggregation-against, anticoagulation, improve many-sided anti thrombotic actions etc. that play such as endothelial function, as adjuvant therapy medicaments in the other system diseases such as breathing, digestion, evident in efficacy.But traditional Chinese medicine is owing to limiting to by preclinical study, continually developing and widespread use along with traditional Chinese medicine in clinical, the report of its bad reaction is also increasing, and therefore improving constantly its quality control level is the necessary means ensureing that product quality is homogeneous, stable.
Traditional Chinese medicine fingerprint adopts the analysis means of various advanced person (technology such as spectrum, wave spectrum, chromatogram) to indicate the characteristic of traditional Chinese medicinal components colony.The Feasible Mode realizing differentiating Chinese medicine authenticity, evaluation quality consistance and product stability, have contain much information, the feature such as characteristic is strong, globality and ambiguity.Finger-print includes the analysis to principal component and non-principal component, the chemical composition information (being embodied in relative retention time and relative peak area) of reflection has high degree of specificity and selectivity, the integral status of various chemical composition amount distribution in Chinese medicine COMPLEX MIXED system can be reflected more fully, especially when present stage, the effective constituent overwhelming majority did not have clear and definite, can in conjunction with various chromatogram, spectrum, wave spectrum means, the true and false of Identification chinese herbs medicine is with good and bad characteristically, becomes " the chemical bar code " of Chinese medicine self.
Chinese patent 201410185466.3 provides a kind of finger print measuring method for the treatment of the traditional Chinese medicine injection of cardiovascular and cerebrovascular disease, the method selects Chinese medicine self component to do reference, only can carry out chromatographic resolution to kind of the composition of 10 in DANHONG ZHUSHEYE and point out, still can not control the quality of DANHONG ZHUSHEYE comprehensively; Document " research of DANHONG ZHUSHEYE finger-print " (the 33rd volume the 8th phase " Chinese patent drug " magazine in 2011), efficient liquid-phase chromatography method is utilized to carry out determining fingerprint pattern to DANHONG ZHUSHEYE, employing protocatechualdehyde is base peak, determine 26 total peaks in collection of illustrative plates, but and fail to point out these total peaks.
Summary of the invention
The problems such as the finger print identifying for prior art existence is imperfect, the invention provides a kind of finger print measuring method of DANHONG ZHUSHEYE, quantitative outer the adding in one in the fingerprint image spectrogram of complexity of the method novelty marks peak, makes the method for foundation accurately easy, highly sensitive, reproducible.
The technical scheme that the present invention is adopted to achieve these goals is:
The invention provides a kind of finger print measuring method of DANHONG ZHUSHEYE, comprise the following steps:
(1) preparation of reference substance solution: take 4,5-Dicaffeoylquinic acid, Rosmarinic acid, Syringin, adenosine, 5 hydroxymethyl furfural, coumaric acid, Kaempferol-O-rutinoside, crocin I, protocatechuic acid, protocatechualdehyde, Sodium Danshensu, caffeic acid reference substance respectively, add acetonitrile respectively to dissolve, make the reference substance solution of 0.1mg/ml respectively;
(2) preparation of inner mark solution: take 4,5-Dicaffeoylquinic acid, adds acetonitrile and makes the inner mark solution that concentration is 1mg/mL;
(3) need testing solution preparation: measure DANHONG ZHUSHEYE, add 0.4% aqueous formic acid dilution, shake up to obtain dilution, get dilution and add the inner mark solution that concentration is 1mg/ml, mixing, to obtain final product;
(4) utilize HPLC MS to carry out analysis to measure.
Further, the preferred preparation method of described need testing solution is: measure DANHONG ZHUSHEYE 5ml, put in 10ml measuring bottle, add 5ml0.4% aqueous formic acid and be diluted to scale, shake up to obtain dilution, get 750 μ l dilutions and add the 4,5-Dicaffeoylquinic acid inner mark solution that 50 μ l concentration are 1mg/mL, mixing, to obtain final product.
Further, described high performance liquid chromatography is separated and uses AgelaVenusilMPC18 chromatographic column: 250mm × 4.6mm, 3 μ L, column temperature 30 DEG C, and flow velocity 1.0mL/min; Determined wavelength 280nm; Under sample size 10 μ L condition, take acetonitrile as mobile phase A, volume fraction is 0.2% aqueous formic acid is Mobile phase B, volume fraction be 0.5% aqueous formic acid be that mobile phase C carries out gradient elution.
Further, the condition of above-mentioned gradient elution is: 0 ~ 4min, 0 ~ 0.3% mobile phase A, 100 ~ 99.7% Mobile phase B; 4 ~ 6min, 0.3 ~ 1.2% mobile phase A, 99.7 ~ 98.8% Mobile phase B; 6 ~ 15min, 1.2 ~ 3% mobile phase A, 98.8 ~ 97% Mobile phase B; 15 ~ 30min, 3 ~ 3% mobile phase A, 97 ~ 97% Mobile phase B; 30 ~ 40min, 3 ~ 5% mobile phase A, 97 ~ 95 Mobile phase B; 40 ~ 60min, 5 ~ 5% mobile phase A, 95 ~ 95% Mobile phase B; 60 ~ 70min, 5 ~ 8% mobile phase A, 95 ~ 92% Mobile phase B; 70 ~ 100min, 8 ~ 8% mobile phase A, 92 ~ 92% Mobile phase B; 100 ~ 125min, 8 ~ 14% mobile phase A, 92 ~ 86% Mobile phase B; 125 ~ 165min, 14 ~ 15.6% mobile phase A, 86 ~ 0% Mobile phase B, 0 ~ 84.4% mobile phase C; 165 ~ 260min, 15.6 ~ 15.6% mobile phase A, 84.4 ~ 84.4% mobile phase C; 260 ~ 272min, 15.6 ~ 16.7% mobile phase A, 84.4 ~ 83.3% mobile phase C; 272 ~ 320min, 16.7 ~ 16.7% mobile phase A, 83.3 ~ 83.3% mobile phase C; 320 ~ 380min, 16.7 ~ 25% mobile phase A, 83.3 ~ 75% mobile phase C; 380 ~ 400min, 25 ~ 25% mobile phase A, 75 ~ 75% mobile phase C;
Described number percent is percent by volume.
Further, the condition of described mass spectroscopy is: electric spray ion source is negative ions alternative scanning mode; Scanning progression 5 grades; Sweep limit: 50 ~ 1000m/z; Sweep velocity 26000m/zs
-1; Spray pressure power 35psi; Dry gas temperature 350 DEG C; Dry gas flow velocity 9Lmin
-1; Capillary voltage 4000V.
Aqueous formic acid used in the present invention is volume fraction.
This method quantitatively adds in one innovatively in the fingerprint image spectrogram of complexity marks peak, adopt the mathematical expression of relative peak area ratio as this finger-print at total peak and interior mark peak, such ratio selects Chinese medicine self component to do the relative peak area at each total peak of reference calculating usually, and the absolute change that more can embody each total peak content changes with relative.
Advantage of the present invention and beneficial effect are:
(1) in gradient elution process, have selected different time sections and select different acid concentration (formic acid of 0.2% and 0.5%) to carry out wash-out, by changing formic acid concn in mobile phase online, good separating effect;
(2) additional internal standard method is selected, test liquid containing internal standard compound matter is carried out to the mensuration of finger-print, adopt the mathematical expression of relative peak area ratio as this finger-print at total peak and interior mark peak, such ratio selects Chinese medicine self component to do the relative peak area at each total peak of reference calculating usually, and the absolute change that more can embody each total peak content changes with relative;
(3) the present invention is directed to design feature and the physicochemical characteristics of effective constituent contained by finished product, the conditions such as need testing solution compound method, mobile phase, elution program, chromatographic column are screened and optimized, the method repeatability selected and good stability;
(4) the present invention can more fully monitor raw medicinal material, semi-manufacture and end product quality, the stability of monitoring production technology.
Accompanying drawing explanation
Fig. 1 is the DANHONG ZHUSHEYE finger-print that embodiment 1 obtains.
Fig. 2 is that the present invention has carried out determining fingerprint pattern to 10 batches of DANHONG ZHUSHEYEs, adopts median method to generate reference fingerprint.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
1.1 instrument
1200 series of high efficiency liquid chromatographic systems (Agilent company of the U.S.), AE240 type electronic analytical balance (Mettler Toledo Inc. of Switzerland), Simplicity pure water instrument (Millipore Corp. of the U.S.).
1.2 reagent
4,5-Dicaffeoylquinic acid reference substance (lot number 14022805), Rosmarinic acid reference substance (lot number 14057812), purchased from Chengdu Purification Technology Development Co., Ltd.; Syringin reference substance (lot number 150120), adenosine reference substance (lot number 141205), 5 hydroxymethyl furfural reference substance (lot number 141227), coumaric acid reference substance (lot number 141224), Kaempferol-O-rutinoside reference substance (lot number 131211), purchased from upper Hiroad standing grain Pharmaceutical Technology Co., Ltd; Crocin I reference substance (lot number MUST-14121204), purchased from Chendu Inst. of Biology, Chinese Academy of Sciences; Protocatechuic acid reference substance (lot number 110809-200102), protocatechualdehyde reference substance (lot number 110810-200506), Sodium Danshensu reference substance (lot number 110855-200405), caffeic acid reference substance (lot number 110885-200102), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
Phase chromatography-use acetonitrile is chromatographically pure, and it is pure that other reagent are analysis.
Test DANHONG ZHUSHEYE is provided by Heze Buchang Pharma Co., Ltd..
embodiment 1
A finger print measuring method for DANHONG ZHUSHEYE, comprises the following steps:
(1) preparation of reference substance solution: take 4,5-Dicaffeoylquinic acid respectively, Rosmarinic acid, Syringin, adenosine, 5 hydroxymethyl furfural, coumaric acid, Kaempferol-O-rutinoside, crocin I, protocatechuic acid, protocatechualdehyde, Sodium Danshensu, caffeic acid reference substance are appropriate, add acetonitrile respectively to dissolve, make the reference substance solution of 0.1mg/ml, keep in Dark Place in 4 DEG C of lower seals;
(2) preparation of inner mark solution: take 4,5-Dicaffeoylquinic acid, adds acetonitrile and makes the inner mark solution that concentration is 1mg/mL;
(3) need testing solution preparation method: precision measures DANHONG ZHUSHEYE 5ml, put in 10ml measuring bottle, adding 5ml volume fraction is that 0.4% aqueous formic acid is diluted to scale, shake up, get 750 μ l dilutions and add 50 μ l 4,5-Dicaffeoylquinic acids inner mark solution (1.0mg/ml), mixing, to obtain final product, test liquid needs matching while using, completes preparation in 30 minutes;
(4) utilize HPLC MS to carry out analysis to measure:
Chromatographic condition: chromatographic column AgelaVenusilMPC18(250mm × 4.6mm, 3 μ L); Mobile phase A: acetonitrile; Mobile phase B: 0.2% formic acid water (v/v); Mobile phase C:0.5% aqueous formic acid (v/v), adopts gradient elution method to carry out wash-out, column temperature 30 DEG C; Flow velocity 1.0mL/min; Determined wavelength 280nm; Sample size 10 μ L, carries out high performance liquid chromatography detection;
The condition of described gradient elution is, specifically sees eluent gradient wash-out table 1.
Table 1 eluent gradient wash-out table
The present invention is to the selection of internal standard compound: having investigated the reference substances such as gallic acid, Chrysophanol, scutelloside, Paeonol, chlorogenic acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, Cryptochlorogenic acid, neochlorogenic acid, galuteolin altogether, to have finally chosen 4,5-Dicaffeoylquinic acid be interior mark; Comparatively other internal standard compounds, through a large amount of tests, applicant finds: the retention time of 4,5-Dicaffeoylquinic acid is about 242min, noiseless, reach baseline separation with adjacent peak, the equal >1.5 of degree of separation of adjacent peak, and be dissolved in test liquid, good stability, the selection difficulty of internal standard compound is large, requires high.
(4) according to the finger print measuring method of above-mentioned foundation, chromatogram is obtained, as shown in Figure 1:
Fingerprint map analyzing is carried out to DANHONG ZHUSHEYE, be with reference to peak (S) with 4,5-Dicaffeoylquinic acid, 26 total peaks are demarcated, total peak area accounts for 94.7% of the total area, by the comparison of reference substance retention time and ultra-violet absorption spectrum, determine wherein 2, 5, 7, 8, 9, 13, 14, 15, 16, 19, No. 20 peaks are respectively adenosine, 5 hydroxymethyl furfural, danshensu, protocatechuic acid, protocatechualdehyde, crocin I, Syringin, caffeic acid, coumaric acid, Kaempferol-O-rutinoside and Rosmarinic acid, (condition of mass spectroscopy is: electric spray ion source to adopt HPLC-MS technology, negative ions alternative scanning mode, scanning progression 5 grades, sweep limit: 50 ~ 1000m/z, sweep velocity 26000m/zs-1, spray pressure power 35psi, dry gas temperature 350 DEG C, dry gas flow velocity 9Lmin-1, capillary voltage 4000V), structure analysis is carried out to the total peak of residue, analysis result is: 6,17,18, No. 26 peaks are respectively danshensu, danshinolic acid H, alkannic acid, salviandic acid A, 21, the quasi-molecular ion peak at 22,24, No. 25 peaks is 717m/z, cracking mode is identical, is danshinolic acid polymer composition.There are 21 peaks at the total peak belonging to the red sage root, be respectively 1-9,12,13,16-18,20-26 peak, there are 5 peaks at the total peak belonging to safflower, be respectively 10,11,14,15, No. 19 peaks, the present invention can carry out finger print identifying to the total peak in 26 DANHONG ZHUSHEYEs, and the total peak retention time of the reference fingerprint of generation is in table 2.
Table 2 DANHONG ZHUSHEYE reference fingerprint has peak and retention time tables of data thereof
1.1 precision test
Get DANHONG ZHUSHEYE need testing solution, continuous sample introduction 6 times, measures according to the method provided in embodiment 1, take 4,5-Dicaffeoylquinic acid as reference, calculates relative peak area and the relative retention time at 26 total peaks.Result shows the equal <1.21% of relative peak area RSD of 26 main peaks, and the equal <1.02% of relative retention time RSD, shows that instrument precision is good.
replica test
Get same lot number DANHONG ZHUSHEYE, the method provided according to embodiment 1 prepares need testing solution, respectively sample introduction 6 times, and record liquid chromatogram take 4,5-Dicaffeoylquinic acid as reference, calculates relative peak area and the relative retention time at 26 total peaks.Result shows the equal <1.8% of relative peak area RSD at 26 total peaks, and the equal <1.2% of relative retention time RSD shows that the repeatability of method is good.
stability test
Get DANHONG ZHUSHEYE need testing solution, the method provided according to embodiment 1, measures in 0,7.2,14.4,21.6,28.8h, take 4,5-Dicaffeoylquinic acid as reference, calculates relative peak area and the relative retention time at 26 total peaks.Result shows the equal <1.5% of relative peak area RSD of 26 main peaks, and the equal <1.33% of relative retention time RSD shows that need testing solution is good at 28.8h internal stability.
According to the method that embodiment 1 provides, determining fingerprint pattern is carried out to 10 batches of DANHONG ZHUSHEYEs, adopted " similarity evaluation (2004A version) ", adopted median method to generate reference fingerprint, see Fig. 2.Each batch sample similarity is all greater than 0.956, and each batch sample is all greater than 0.972 with the collection of illustrative plates similarity that contrasts of generation, and concrete outcome is in table 3.
Table 310 batch DANHONG ZHUSHEYE fingerprint chromatogram Similarity Measure result
As shown in Table 3, each batch sample similarity is all greater than 0.956, and each batch sample contrasts trace analysis with generation, and similarity is all greater than 0.972.Show that DANHONG ZHUSHEYE technique is relatively stable, product homogeneity is better, carries out quality control more reliable by the method to DANHONG ZHUSHEYE.
Claims (5)
1. a finger print measuring method for DANHONG ZHUSHEYE, is characterized in that, comprises the following steps:
(1) preparation of reference substance solution: take 4,5-Dicaffeoylquinic acid, Rosmarinic acid, Syringin, adenosine, 5 hydroxymethyl furfural, coumaric acid, Kaempferol-O-rutinoside, crocin I, protocatechuic acid, protocatechualdehyde, Sodium Danshensu, caffeic acid reference substance respectively, add acetonitrile respectively to dissolve, make the reference substance solution of 0.1mg/ml respectively;
(2) preparation of inner mark solution: take 4,5-Dicaffeoylquinic acid, adds acetonitrile and makes the inner mark solution that concentration is 1mg/mL;
(3) need testing solution preparation: measure DANHONG ZHUSHEYE, add 0.4% aqueous formic acid dilution, shake up to obtain dilution, get dilution and add the inner mark solution that concentration is 1mg/ml, mixing, to obtain final product;
(4) utilize HPLC MS to carry out analysis to measure.
2. finger print measuring method according to claim 1, it is characterized in that, the preparation method of described need testing solution is: measure DANHONG ZHUSHEYE 5ml, put in 10ml measuring bottle, add 5ml0.4% aqueous formic acid and be diluted to scale, shake up to obtain dilution, get 750 μ l dilutions and add the 4,5-Dicaffeoylquinic acid inner mark solution that 50 μ l concentration are 1mg/mL, mixing, to obtain final product.
3. finger print measuring method according to claim 1 and 2, is characterized in that, described high performance liquid chromatography is separated and uses AgelaVenusilMPC18 chromatographic column: 250mm × 4.6mm, 3 μ L, column temperature 30 DEG C, and flow velocity 1.0mL/min; Determined wavelength 280nm; Under sample size 10 μ L condition, take acetonitrile as mobile phase A, volume fraction is 0.2% aqueous formic acid is Mobile phase B, volume fraction be 0.5% aqueous formic acid be that mobile phase C carries out gradient elution.
4. finger print measuring method according to claim 3, is characterized in that, the condition of described gradient elution is: 0 ~ 4min, 0 ~ 0.3% mobile phase A, 100 ~ 99.7% Mobile phase B; 4 ~ 6min, 0.3 ~ 1.2% mobile phase A, 99.7 ~ 98.8% Mobile phase B; 6 ~ 15min, 1.2 ~ 3% mobile phase A, 98.8 ~ 97% Mobile phase B; 15 ~ 30min, 3 ~ 3% mobile phase A, 97 ~ 97% Mobile phase B; 30 ~ 40min, 3 ~ 5% mobile phase A, 97 ~ 95 Mobile phase B; 40 ~ 60min, 5 ~ 5% mobile phase A, 95 ~ 95% Mobile phase B; 60 ~ 70min, 5 ~ 8% mobile phase A, 95 ~ 92% Mobile phase B; 70 ~ 100min, 8 ~ 8% mobile phase A, 92 ~ 92% Mobile phase B; 100 ~ 125min, 8 ~ 14% mobile phase A, 92 ~ 86% Mobile phase B; 125 ~ 165min, 14 ~ 15.6% mobile phase A, 86 ~ 0% Mobile phase B, 0 ~ 84.4% mobile phase C; 165 ~ 260min, 15.6 ~ 15.6% mobile phase A, 84.4 ~ 84.4% mobile phase C; 260 ~ 272min, 15.6 ~ 16.7% mobile phase A, 84.4 ~ 83.3% mobile phase C; 272 ~ 320min, 16.7 ~ 16.7% mobile phase A, 83.3 ~ 83.3% mobile phase C; 320 ~ 380min, 16.7 ~ 25% mobile phase A, 83.3 ~ 75% mobile phase C; 380 ~ 400min, 25 ~ 25% mobile phase A, 75 ~ 75% mobile phase C;
Described number percent is percent by volume.
5. finger print measuring method according to claim 1, is characterized in that, the condition of described mass spectroscopy is: electric spray ion source is negative ions alternative scanning mode; Scanning progression 5 grades; Sweep limit: 50 ~ 1000m/z; Sweep velocity 26000m/zs
-1; Spray pressure power 35psi; Dry gas temperature 350 DEG C; Dry gas flow velocity 9Lmin
-1; Capillary voltage 4000V.
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| CN106680410A (en) * | 2017-02-17 | 2017-05-17 | 南京中医药大学 | Screening method for research on compatibility stability of traditional Chinese medicine injection and solvent |
| CN106770701A (en) * | 2016-11-16 | 2017-05-31 | 天津中医药大学 | The assay method of Danshen injection Polyphenol Acids active ingredient |
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| CN117233306A (en) * | 2023-11-16 | 2023-12-15 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117233306A (en) * | 2023-11-16 | 2023-12-15 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
| CN117233306B (en) * | 2023-11-16 | 2024-01-30 | 江西省药品检验检测研究院 | Fingerprint establishment and component content determination method for jindan Fuyan particles |
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