CN102133333B - Quality control method for shenmai injection mass spectrum finger prints - Google Patents
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- 239000008862 fructus schizandrae, radix ginseng, radix ophiopogonis drug combination Substances 0.000 title claims abstract description 80
- 238000002347 injection Methods 0.000 title claims abstract description 79
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- 238000001819 mass spectrum Methods 0.000 title claims abstract description 48
- 238000003908 quality control method Methods 0.000 title abstract description 10
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- 238000000034 method Methods 0.000 claims abstract description 16
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 52
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Abstract
The invention provides a quality control method for shenmai injection mass spectrum finger prints. Liquid chromatogram is adopted as a separation measure, and a mass spectrum detector is taken as a detection measure so as to obtain two finger prints for representing compound information of red ginseng and radix ophiopogonis in shenmai injection; and the similarity is calculated by adopting a correlation coefficient method, and samples with the similarity more than or equal to 0.9 are judged as products with stable quality. In the quality control method, the characteristics that the mass spectrum detector has high sensitivity and strong specificity, and can sample in multiple channels are utilized, and a method for detecting in the multiple channels and with different modes is selected, so that the two finger prints can be obtained by one-time analysis, the compound information of red ginseng and radix ophiopogonis in a preparation can be reflected simultaneously, the completeness and the specificity of the information of the finger prints of the preparation are ensured, the repeatability is good, and the technical guarantee is provided for the quality control of the shenmai injection.
Description
Technical field
The invention belongs to the fingerprint map analyzing technical field, particularly a kind of quality control method for shenmai injection mass spectrum finger prints.
Background technology
Finger-print is a kind of methodology of studying on the whole the complex material system.At the traditional Chinese medicine quality control field, because the existing method of measuring one or several chemical composition content can not be made accurate evaluation to the Chinese medicine total quality, be difficult to reach according to " amount " purpose of control " matter ", fingerprint pattern technology is because of its globality and ambiguity, caused researchist's extensive concern in the industry, by the mechanisms such as U.S. FDA, state food and Drug Administration accept extensively for estimate autonomic drug or Chinese medicine batch between quality stability.At present, the traditional Chinese medicine fingerprint technology mainly adopts high performance liquid chromatography, gas chromatography isochromatic spectrum analytical approach to obtain the sample analysis spectrogram, carries out qualitative analysis.
Shenmai injection comes from traditional Chinese medicine recipe " Shengmai San ", is comprised of the Chinese medicine of distinguishing the flavor of red ginseng and the tubers of dwarf lilyturf two.Red ginseng is the dry root and rhizome of cultivation product after steaming of Araliaceae ginseng, has and reinforces vital energy, and beneficial blood, the effect of mental-tranquilization, be the Liliaceae Ophiopogon tuber of dwarf lilyturf, is the enriching yin Chinese medicine of commonly using, and has function promoting production of body fluid and nourishing the lung, replenishing the vital essence and removing heat.Shenmai injection curative effect in angiocardiopathy and tumor aid treatment is clear and definite, and has obtained clinical practice widely.In red ginseng, main effective constituent is the ginsenoside compounds, and in the tuber of dwarf lilyturf, main effective constituent is ophiopogonin class and flavone compound.Saponins compound all only has absorption at the ultraviolet end.In preparation, the ginsenoside kind compound content is higher, and the tuber of dwarf lilyturf, chemical composition content was lower.Existing research adopts high-efficient liquid phase chromatogram technology to carry out the Shenmai injection fingerprint map analyzing take ultraviolet or evaporative light-scattering detector as detection means, has mainly reflected ginsenoside compounds information in spectrogram, and the tuber of dwarf lilyturf, composition embodied not enough.If with the tuber of dwarf lilyturf composition also include the Quality Control scope in, will be conducive to promote the quality control standard of Shenmai injection, further ensure the quality stability of this product.
Summary of the invention
The present invention is directed to above-mentioned technical need, a kind of quality control method for shenmai injection mass spectrum finger prints is provided, realize by following steps: the employing liquid chromatography is separation means, obtain simultaneously two kinds of LC-MS (LC/MS) finger-print of red ginseng and tuber of dwarf lilyturf compound information in the Shenmai injection of at least 10 batches of signs take mass detector as detection means, adopt correlation coefficient process to calculate the similarity of each batch, the sample of Xiang Si Du＞=0.9 is evaluated as stay-in-grade product.
Concrete steps are as follows:
(1) for the preparation of trial product solution
Get respectively more than 10 batches Shenmai injection appropriate, 10000 turn/centrifugal 10 min of min, get supernatant standby.
(2) obtain finger-print I and II
With standby supernatant, by LC-MS (LC/MS), obtain respectively finger-print,
A. chromatographic condition
Adopt C
18The fast liquid chromatography post of bonding (100 mm * 4.6 mm i.d., 1.8 μ m), mobile phase is 0.06% aqueous formic acid A and acetonitrile B, the gradient elution program is: 0～10 min, 5～15% B; 10～25 min, 15～25% B; 25～30 min, 25～30% B; 30～45 min, 30～35% B; 45～50 min, 35～45% B; 50～70 min, 45～70% B; 70～75 min, 70～90% B, column temperature: 30 ℃, sample size: 5 μ l.
B. the mass spectrum condition of finger-print I
Nitrogen temperature: 250 ~ 350 ℃; Atomizing pressure: 40 ~ 50 psi; Nitrogen flow rate: 9 ~ 12 L/min; Capillary voltage: 2500 ~ 4000 V; Cracking voltage in the source: 250 V; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Best mass spectrum condition is: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Cracking voltage in the source: 250 V; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400.
C. finger-print II mass spectrum condition
nitrogen temperature: 250 ~ 350 ℃, atomizing pressure: 40 ~ 50 psi, nitrogen flow rate: 9 ~ 12 L/min, capillary voltage: 2500 ~ 4000 V, negative ion is selected the ion detection pattern, select altogether the ion of 64 kinds of different m/z, select the m/z of ion to be: 233, 249, 301, 309, 313, 319, 327, 329, 337, 339, 341, 351, 353, 355, 359, 369, 375, 409, 411, 419, 445, 447, 477, 493, 515, 519, 533, 563, 565, 567, 641, 667, 675, 681, 685, 715, 737, 753, 767, 787, 833, 835, 839, 853, 863, 869, 885, 899, 915, 931, 953, 961, 987, 1031, 1047, 1061, 1063, 1093, 1095, 1135, 1255, 1257, 1271, cracking voltage in the source: 100 ~ 350 V, each selects cracking voltage in ion pair should be separately best source.
best mass spectrum condition is: nitrogen temperature: 350 ℃, atomizing pressure: 45 psi, nitrogen flow rate: 11 L/min, capillary voltage: 3500 V, negative ion is selected the ion detection pattern, select altogether the ion of 64 kinds of different m/z, select the m/z of ion to be: 233, 249, 301, 309, 313, 319, 327, 329, 337, 339, 341, 351, 353, 355, 359, 369, 375, 409, 411, 419, 445, 447, 477, 493, 515, 519, 533, 563, 565, 567, 641, 667, 675, 681, 685, 715, 737, 753, 767, 787, 833, 835, 839, 853, 863, 869, 885, 899, 915, 931, 953, 961, 987, 1031, 1047, 1061, 1063, 1093, 1095, 1135, 1255, 1257, 1271, cracking voltage range in the source: 100 ~ 350 V, each selects cracking voltage in ion pair should be separately best source.
3. quality stability evaluation
With Shenmai injection finger-print I and the II more than 10 batches of obtaining, be fused into a finger-print with serial mode respectively, take all batches sample average as standard finger-print, adopt correlation coefficient process to calculate the similarity of each batch, the sample of Xiang Si Du＞=0.9 is evaluated as stay-in-grade product.
Usefulness of the present invention: adopt the LC-MS technology to carry out the Shenmai injection fingerprint map analyzing, utilize that mass detector is highly sensitive, specificity is strong, characteristics that can multi-channel sampling, by the method for selecting the hyperchannel different mode to detect, once analyze and to obtain two kinds of finger-prints.The compound information that reflects simultaneously two kinds of medicinal materials of red ginseng and the tuber of dwarf lilyturf in preparation.Shenmai injection finger-print information integrity and specificity have been guaranteed, for the Shenmai injection quality control provides good technical guarantee.The method has good reappearance, and in finger-print, each total peak retention time RSD is less than 0.11%, and unimodal area accounts for the total peak-to-peak area RSD of total peak area 2 ﹪ less than 4.9 %.
Description of drawings
The different nitrogen temperature Shenmai injection of Fig. 1 finger-print I total ion current figure.
The different capillary voltage Shenmai injection of Fig. 2 finger-print I total ion current figure.
The different nitrogen flow rate Shenmai injection of Fig. 3 finger-print I total ion current figure.
The different atomizing pressure Shenmai injection of Fig. 4 finger-print I total ion current figure.
Fig. 5 Shenmai injection finger-print I total ion current figure.
The different nitrogen temperature Shenmai injection of Fig. 6 finger-print II is always selected the ion flow graph.
The different capillary voltage Shenmai injection of Fig. 7 finger-print II is always selected the ion flow graph.
The different nitrogen flow rate Shenmai injection of Fig. 8 finger-print II is always selected the ion flow graph.
The different atomizing pressure Shenmai injection of Fig. 9 finger-print II is always selected the ion flow graph.
Figure 10 Shenmai injection finger-print II is always selected the ion flow graph.
Figure 11 Shenmai injection similarity evaluation result (n=20, similarity is all greater than 0.9).
Figure 12 Shenmai injection similarity evaluation result (n=10,, similarity is all greater than 0.9).
Embodiment
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing.
1. need testing solution preparation
Get Shenmai injection appropriate, 10000 turn/centrifugal 10 min of min, get supernatant standby;
2. Shenmai injection LC/MS finger-print I chromatographic condition
Adopt C
18The fast liquid chromatography post Edipse Plus C of bonding
18(100 mm * 4.6 mm i.d., 1.8 μ m), mobile phase is 0.06% aqueous formic acid A and acetonitrile B, the gradient elution program is: 0～10 min, 5～15% B; 10～25 min, 15～25% B; 25～30 min, 25～30% B; 30～45 min, 30～35% B; 45～50 min, 35～45% B; 50～70 min, 45～70% B; 70～75 min, 70～90% B, column temperature: 30 ℃, sample size: 5 μ l;
3. Shenmai injection LC/MS finger-print I mass spectrum condition
Atomizing pressure: 45 psi; Nitrogen flow rate: 12 L/min; Capillary voltage: 3000 V; Cracking voltage in the source: 250 V; Nitrogen temperature: 250,300 and 350 ℃; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 1, different nitrogen temperature Shenmai injection finger-print I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, difference is the mass spectrum condition.Mass spectrum condition: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 12 L/min; Cracking voltage in the source: 250 V; Capillary voltage: 2500,3000,3500 and 4000 V; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 2, different capillary voltage Shenmai injection finger-print I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, difference is the mass spectrum condition.
Mass spectrum condition: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Cracking voltage in the source: 250 V; Capillary voltage: 3500; Nitrogen flow rate: 9,10,11,12 L/min; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 3, different nitrogen flow rate Shenmai injection finger-print I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, difference is the mass spectrum condition.
Mass spectrum condition: nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Cracking voltage in the source: 250 V; Capillary voltage: 3500; Atomizing pressure: 40,45 and 50psi; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 4, different atomizing pressure Shenmai injection finger-print I total ion current figure.
Under the best mass spectrum condition of embodiment 5, Shenmai injection finger-print I is analyzed
Need testing solution preparation and chromatographic condition such as embodiment 1, difference is the mass spectrum condition.
Mass spectrum condition: nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Cracking voltage in the source: 250 V; Capillary voltage: 3500; Atomizing pressure: 45 psi; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 5, Shenmai injection finger-print I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, difference is the mass spectrum condition.
Mass spectrum condition: atomizing pressure: 45 psi; Nitrogen flow rate: 12 L/min; Capillary voltage: 3000 V; Cracking voltage in the source: 250 V; Nitrogen temperature: 250,300 and 350 ℃; Negative ion is selected the ion detection pattern, and in selection ion m/z and corresponding source thereof, cracking voltage sees Table 1.
Analysis result is seen accompanying drawing 6, and different nitrogen temperature Shenmai injection finger-print II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and corresponding source thereof, difference is other mass spectrum conditions.
Other mass spectrum conditions: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 12 L/min; Capillary voltage: 2500,3000,3500 and 4000 V.
Analysis result is seen accompanying drawing 7, and different capillary voltage Shenmai injection finger-print II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and corresponding source thereof, difference is other mass spectrum conditions.
Other mass spectrum conditions: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Capillary voltage: 3500; Nitrogen flow rate: 9,10,11,12 L/min.
Analysis result is seen accompanying drawing 8, and different nitrogen flow rate Shenmai injection finger-print II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and corresponding source thereof, difference is other mass spectrum conditions.
Other mass spectrum conditions: nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500; Atomizing pressure: 40,45 and 50psi.
Analysis result is seen accompanying drawing 9, and different atomizing pressure Shenmai injection finger-print II are always selected the ion flow graph.
Under the best mass spectrum condition of embodiment 10, Shenmai injection finger-print II is analyzed
Detecting pattern in need testing solution preparation, chromatographic condition and mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and corresponding source thereof, difference is other mass spectrum conditions.
Other mass spectrum conditions: nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500; Atomizing pressure: 45 psi.
Analysis result is seen accompanying drawing 10, and Shenmai injection finger-print II is always selected the ion flow graph.
Choose 20 batches of Shenmai injections that 2007-2010 produces, carry out Shenmai injection finger-print I and II analysis, obtain its LC/MS finger-print, be fused into a finger-print with serial mode respectively; And take all batches sample average as standard finger-print, adopt correlation coefficient process to calculate its similarity.Similarity evaluation result such as Figure 11, result shows 20 batches of Shenmai injection similarities all greater than 0.9, shows that between Shenmai injection batch, quality stability is good.The specific implementation method of serial mode see document (Fan Xiaohui, Ye Zhengliang, Cheng Yiyu. based on the Chinese medicine multiple elements chemical finger-print similarity calculation method of information fusion, SCI. 2006,27 (1): 26-29).
Shenmai injection finger-print I and II analytical approach:
1. need testing solution preparation
Get Shenmai injection appropriate, 10000 turn/centrifugal 10 min of min, get supernatant standby;
2. the chromatographic condition of Shenmai injection LC/MS finger-print I and II
Adopt C
18The fast liquid chromatography post Edipse Plus C of bonding
18(100 mm * 4.6 mm i.d., 1.8 μ m), mobile phase is 0.06% aqueous formic acid A and acetonitrile B, the gradient elution program is: 0～10 min, 5～15% B; 10～25 min, 15～25% B; 25～30 min, 25～30% B; 30～45 min, 30～35% B; 45～50 min, 35～45% B; 50～70 min, 45～70% B; 70～75 min, 70～90% B, column temperature: 30 ℃, sample size: 5 μ l;
3. Shenmai injection LC/MS finger-print I mass spectrum condition
Nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Cracking voltage in the source: 250 V; Capillary voltage: 3500; Atomizing pressure: 45 psi; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
4. Shenmai injection LC/MS finger-print II mass spectrum condition
Nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Negative ion is selected the ion detection pattern, and in the m/z of 64 kinds of selection ions and each self-corresponding source, cracking voltage sees Table 1.
Choose 10 batches of Shenmai injections of production in 2010, carry out Shenmai injection finger-print I and II analysis, obtain its LC/MS finger-print, be fused into a finger-print with serial mode respectively; And take all batches sample average as standard finger-print, adopt correlation coefficient process to calculate its similarity.Similarity evaluation result such as Figure 12, result shows 10 batches of Shenmai injection similarities all greater than 0.9, shows that between Shenmai injection batch, quality stability is good.The specific implementation method of serial mode see document (Fan Xiaohui, Ye Zhengliang, Cheng Yiyu. based on the Chinese medicine multiple elements chemical finger-print similarity calculation method of information fusion, SCI. 2006,27 (1): 26-29).
Shenmai injection finger-print I and II analytical approach:
1. need testing solution preparation
Get Shenmai injection appropriate, 10000 turn/centrifugal 10 min of min, get supernatant standby;
2. the chromatographic condition of Shenmai injection LC/MS finger-print I and II
Adopt C
18The fast liquid chromatography post Edipse Plus C of bonding
18(100 mm * 4.6 mm i.d., 1.8 μ m), mobile phase is 0.06% aqueous formic acid A and acetonitrile B, the gradient elution program is: 0～10 min, 5～15% B; 10～25 min, 15～25% B; 25～30 min, 25～30% B; 30～45 min, 30～35% B; 45～50 min, 35～45% B; 50～70 min, 45～70% B; 70～75 min, 70～90% B, column temperature: 30 ℃, sample size: 5 μ l;
3. Shenmai injection LC/MS finger-print I mass spectrum condition
Nitrogen temperature: 350 ℃; Nitrogen flow rate: 11 L/min; Cracking voltage in the source: 250 V; Capillary voltage: 3500; Atomizing pressure: 45 psi; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
4. Shenmai injection LC/MS finger-print II mass spectrum condition
Nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Negative ion is selected the ion detection pattern, and in the m/z of 64 kinds of selection ions and each self-corresponding source, cracking voltage sees Table 1.
Claims (2)
1. a Shenmai injection mass spectrum fingerprint pattern quality determining method, is characterized in that, realizes by following steps:
(1) for the preparation of trial product solution
Get Shenmai injection more than 10 batches, carry out respectively 10000 and turn/centrifugal 10 min of min, get supernatant standby;
(2) obtain finger-print I and II
With standby supernatant, by LC-MS, obtain respectively finger-print,
A. chromatographic condition
Adopt C
18The fast liquid chromatography post of bonding, 100 mm * 4.6 mm i.d., 1.8 μ m, mobile phase are 0.06% aqueous formic acid A and acetonitrile B, the gradient elution program is: 0～10 min, 5～15% B; 10～25 min, 15～25% B; 25～30 min, 25～30% B; 30～45 min, 30～35% B; 45～50 min, 35～45% B; 50～70 min, 45～70% B; 70～75 min, 70～90% B, column temperature: 30 ℃, sample size: 5 μ l;
B. the mass spectrum condition of finger-print I
Nitrogen temperature: 250 ~ 350 ℃; Atomizing pressure: 40 ~ 50 psi; Nitrogen flow rate: 9 ~ 12 L/min; Capillary voltage: 2500 ~ 4000 V; Cracking voltage in the source: 250 V; Negative ion scanning detecting pattern, scanning m/z scope: 200-1400;
C. finger-print II mass spectrum condition
the mass spectrum condition is: nitrogen temperature: 250 ~ 350 ℃, atomizing pressure: 40 ~ 50 psi, nitrogen flow rate: 9 ~ 12 L/min, capillary voltage: 2500 ~ 4000 V, negative ion is selected the ion detection pattern, select altogether the ion of 64 kinds of different m/z, select the m/z of ion to be: 233, 249, 301, 309, 313, 319, 327, 329, 337, 339, 341, 351, 353, 355, 359, 369, 375, 409, 411, 419, 445, 447, 477, 493, 515, 519, 533, 563, 565, 567, 641, 667, 675, 681, 685, 715, 737, 753, 767, 787, 833, 835, 839, 853, 863, 869, 885, 899, 915, 931, 953, 961, 987, 1031, 1047, 1061, 1063, 1093, 1095, 1135, 1255, 1257, 1271, cracking voltage range in the source: 100 ~ 350 V, each selects cracking voltage in ion pair should be separately best source,
(3) quality stability detects
Get Shenmai injection finger-print I and the II more than 10 batches obtained, be fused into a finger-print with serial mode respectively, take all batches sample average as standard finger-print, the employing correlation coefficient process calculates the similarity of each batch, by the quality stability of similarity test sample.
2. a kind of Shenmai injection mass spectrum fingerprint pattern quality determining method according to claim 1, it is characterized in that, the mass spectrum condition of step (2) b finger-print I is: nitrogen temperature: 350 ℃, atomizing pressure: 45 psi, nitrogen flow rate: 11 L/min, capillary voltage: 3500 V, cracking voltage in the source: 250 V, negative ion scanning detecting pattern, scanning m/z scope: 200-1400.
3. a kind of Shenmai injection mass spectrum fingerprint pattern quality determining method according to claim 1, is characterized in that, the mass spectrum condition of step (2) c finger-print II is: nitrogen temperature: 350 ℃, atomizing pressure: 45 psi, nitrogen flow rate: 11 L/min, capillary voltage: 3500 V, negative ion is selected the ion detection pattern, select altogether the ion of 64 kinds of different m/z, select the m/z of ion to be: 233, 249, 301, 309, 313, 319, 327, 329, 337, 339, 341, 351, 353, 355, 359, 369, 375, 409, 411, 419, 445, 447, 477, 493, 515, 519, 533, 563, 565, 567, 641, 667, 675, 681, 685, 715, 737, 753, 767, 787, 833, 835, 839, 853, 863, 869, 885, 899, 915, 931, 953, 961, 987, 1031, 1047, 1061, 1063, 1093, 1095, 1135, 1255, 1257, 1271, cracking voltage range in the source: 100 ~ 350 V, each selects cracking voltage in ion pair should be separately best source.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110073973 CN102133333B (en) | 2011-03-25 | 2011-03-25 | Quality control method for shenmai injection mass spectrum finger prints |
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| CN102680626A (en) * | 2012-05-09 | 2012-09-19 | 正大青春宝药业有限公司 | Quantitative detection method for characteristic components in Shenmai injection |
| CN102692462B (en) * | 2012-06-03 | 2014-01-08 | 浙江大学 | Danhong injection quality control method |
| CN103837609B (en) * | 2012-11-26 | 2016-08-03 | 华润三九（雅安）药业有限公司 | A kind of SHENGMAI ZHUSHEYE and preparation method thereof |
| CN103728332B (en) * | 2014-01-24 | 2016-08-17 | 西南民族大学 | A kind of discrimination method of Shenmai injection end product quality |
| CN111366672B (en) * | 2020-04-24 | 2021-06-22 | 劲牌有限公司 | Detection method of health wine fingerprint |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
| CN1939501A (en) * | 2005-09-29 | 2007-04-04 | 北京华医神农医药科技有限公司 | Ginseng glucose injection and its quality control |
| CN101375990A (en) * | 2007-08-29 | 2009-03-04 | 济南天瑞本草医药科技有限公司 | Composition for treating cardiovascular disease and preparation thereof |
-
2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
| CN1939501A (en) * | 2005-09-29 | 2007-04-04 | 北京华医神农医药科技有限公司 | Ginseng glucose injection and its quality control |
| CN101375990A (en) * | 2007-08-29 | 2009-03-04 | 济南天瑞本草医药科技有限公司 | Composition for treating cardiovascular disease and preparation thereof |
Non-Patent Citations (4)
| Title |
|---|
| 制备工艺对参麦注射液质量的影响;吴永江等;《中国中药杂志》;20050920(第09期);663-665 * |
| 吴永江等.制备工艺对参麦注射液质量的影响.《中国中药杂志》.2005,(第09期), |
| 陈闽军等.高效液相色谱用于参麦注射液人参皂苷的含量测定和批次一致性考察.《中国药学杂志》.2003,(第08期), |
| 高效液相色谱用于参麦注射液人参皂苷的含量测定和批次一致性考察;陈闽军等;《中国药学杂志》;20030815(第08期);623-626 * |
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