CN102133333A - Quality control method for shenmai injection mass spectrum finger prints - Google Patents
Quality control method for shenmai injection mass spectrum finger prints Download PDFInfo
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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 SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control.
Background technology
Finger printing is a kind of methodology of studying the complex material system on the whole.In 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 the purpose of control " matter " according to " amount ", fingerprint pattern technology is because of its globality and ambiguity, caused the extensive concern of research worker in the industry, by mechanisms such as U.S. FDA, state food and Drug Administration accept extensively be used to estimate plant amedica or Chinese medicine batch between quality stability.At present, the Chinese medicine fingerprint technology mainly adopts high performance liquid chromatography, gas chromatogram isochromatic spectrum analytical method to obtain the sample analysis spectrogram, carries out qualitative analysis.
SHENMAI ZHUSHEYE comes from Chinese medicine name side " SHENGMAI SAN ", is made up of the Chinese medicine of distinguishing the flavor of Radix Ginseng Rubra and Radix Ophiopogonis two.Radix Ginseng Rubra is the dry root and rhizome of cultivation product after steaming of Araliaceae Radix Ginseng, has strongly invigorating primordial QI, beneficial blood, and the effect of tranquilizing by nourishing the heart, be the Liliaceae Ophiopogon Radix Ophiopogonis, is the YIN nourishing Chinese medicine of using always, has the function of promoting the production of body fluid for nourishing the lung, replenishing YIN and removing heat.SHENMAI ZHUSHEYE curative effect in cardiovascular disease and tumor aid treatment is clear and definite, and has obtained clinical practice widely.Main effective ingredient is ginsenoside's compounds in the Radix Ginseng Rubra, and main effective ingredient is ophiopogonin class and flavone compound in Radix Ophiopogonis.Saponins compound all only has absorption at the ultraviolet end.Ginsenoside's kind compound content is higher in the preparation, and Radix Ophiopogonis, chemical composition content was lower.It is that detection means is carried out the SHENMAI ZHUSHEYE fingerprint map analyzing with ultraviolet or evaporative light scattering detector that high-efficient liquid phase chromatogram technology is adopted in existing research, has mainly reflected ginsenoside's compounds information in the spectrogram, and Radix Ophiopogonis, composition embodied not enough.If can also include composition Radix Ophiopogonis in the Quality Control scope, will help promoting the quality control standard of SHENMAI ZHUSHEYE, further ensure this product quality stability.
Summary of the invention
The present invention is directed to above-mentioned technical need, a kind of SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control is provided, realize by following steps: the employing liquid chromatograph is a separation means, it with the mass detector two kinds of LC-MS (LC/MS) finger printing that detection means is obtained Radix Ginseng Rubra and Radix Ophiopogonis chemical compound information in the SHENMAI ZHUSHEYE of at least 10 batches of signs simultaneously, 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 trial product formulations prepared from solutions
It is an amount of to get more than 10 batches SHENMAI ZHUSHEYE respectively, centrifugal 10 min of 10000 commentaries on classics/min, and it is standby to get supernatant.
(2) obtain finger printing I and II
With standby supernatant, by LC-MS (LC/MS), obtain finger printing respectively,
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 printing 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; Anion 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400.
C. finger printing 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; Anion is selected the ion detection pattern, select the ion of 64 kinds of different m/z altogether, select ionic m/z 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 should be the separately best source of ion pair.
Best mass spectrum condition is: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Anion is selected the ion detection pattern, select the ion of 64 kinds of different m/z altogether, select ionic m/z 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 should be the separately best source of ion pair.
3. quality stability evaluation
With SHENMAI ZHUSHEYE finger printing I and the II of obtaining more than 10 batches, be fused into a finger printing with serial mode respectively, with all batches sample average is 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 ZHUSHEYE 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 multichannel different mode to detect, once analyze and to obtain two kinds of finger printing.The chemical compound information that reflects two kinds of medical materials of Radix Ginseng Rubra and Radix Ophiopogonis in the preparation simultaneously.SHENMAI ZHUSHEYE finger printing information integrity and specificity have been guaranteed, for the SHENMAI ZHUSHEYE quality control provides good technical guarantee.This method has good repeatability, and each total peak retention time RSD is less than 0.11% in the finger printing, 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 ZHUSHEYE of Fig. 1 finger printing I total ion current figure.
The different capillary voltage SHENMAI ZHUSHEYE of Fig. 2 finger printing I total ion current figure.
The different nitrogen flow rate SHENMAI ZHUSHEYE of Fig. 3 finger printing I total ion current figure.
The different atomizing pressure SHENMAI ZHUSHEYE of Fig. 4 finger printing I total ion current figure.
Fig. 5 SHENMAI ZHUSHEYE finger printing I total ion current figure.
The different nitrogen temperature SHENMAI ZHUSHEYE of Fig. 6 finger printing II is always selected the ion flow graph.
The different capillary voltage SHENMAI ZHUSHEYE of Fig. 7 finger printing II is always selected the ion flow graph.
The different nitrogen flow rate SHENMAI ZHUSHEYE of Fig. 8 finger printing II is always selected the ion flow graph.
The different atomizing pressure SHENMAI ZHUSHEYE of Fig. 9 finger printing II is always selected the ion flow graph.
Figure 10 SHENMAI ZHUSHEYE finger printing II is always selected the ion flow graph.
Figure 11 SHENMAI ZHUSHEYE similarity evaluation result (n=20, similarity is all greater than 0.9).
Figure 12 SHENMAI ZHUSHEYE similarity evaluation result (n=10,, similarity is all greater than 0.9).
The specific embodiment
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing.
1. need testing solution preparation
It is an amount of to get SHENMAI ZHUSHEYE, centrifugal 10 min of 10000 commentaries on classics/min, and it is standby to get supernatant;
2. SHENMAI ZHUSHEYE LC/MS finger printing 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 ZHUSHEYE LC/MS finger printing 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 ℃; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 1, different nitrogen temperature SHENMAI ZHUSHEYE finger printing I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, different 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 2, different capillary voltage SHENMAI ZHUSHEYE finger printing I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, different 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 3, different nitrogen flow rate SHENMAI ZHUSHEYE finger printing I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, different 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 4, different atomizing pressure SHENMAI ZHUSHEYE finger printing I total ion current figure.
SHENMAI ZHUSHEYE finger printing I is analyzed under the embodiment 5 best mass spectrum conditions
Need testing solution preparation and chromatographic condition such as embodiment 1, different 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
Analysis result is seen accompanying drawing 5, SHENMAI ZHUSHEYE finger printing I total ion current figure.
Need testing solution preparation and chromatographic condition such as embodiment 1, different 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 ℃; Anion is selected the ion detection pattern, and cracking voltage sees Table 1 in selection ion m/z and the corresponding source thereof.
Analysis result is seen accompanying drawing 6, and different nitrogen temperature SHENMAI ZHUSHEYE finger printing II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and the mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and the corresponding source thereof, different 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 ZHUSHEYE finger printing II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and the mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and the corresponding source thereof, different 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 ZHUSHEYE finger printing II are always selected the ion flow graph.
Detecting pattern in need testing solution preparation, chromatographic condition and the mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and the corresponding source thereof, different 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 ZHUSHEYE finger printing II are always selected the ion flow graph.
SHENMAI ZHUSHEYE finger printing II is analyzed under the embodiment 10 best mass spectrum conditions
Detecting pattern in need testing solution preparation, chromatographic condition and the mass spectrum condition, select cracking voltage such as embodiment 6 in ion m/z and the corresponding source thereof, different 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 ZHUSHEYE finger printing II is always selected the ion flow graph.
Choose 20 batches of SHENMAI ZHUSHEYE that 2007-2010 produces, carry out SHENMAI ZHUSHEYE finger printing I and II analysis, obtain its LC/MS finger printing, be fused into a finger printing with serial mode respectively; And be standard finger-print with all batches sample average, adopt correlation coefficient process to calculate its similarity.Similarity evaluation result such as Figure 11, result show 20 batches of SHENMAI ZHUSHEYE similarities all greater than 0.9, show that quality stability is good between SHENMAI ZHUSHEYE batch.The specific implementation method of serial mode see document (Fan Xiaohui, Ye Zhengliang, Cheng Yiyu. based on the Chinese medicine multiple elements chemical finger printing similarity calculation method of information fusion, SCI. 2006,27 (1): 26-29).
SHENMAI ZHUSHEYE finger printing I and II analytical method:
1. need testing solution preparation
It is an amount of to get SHENMAI ZHUSHEYE, centrifugal 10 min of 10000 commentaries on classics/min, and it is standby to get supernatant;
2. the chromatographic condition of SHENMAI ZHUSHEYE LC/MS finger printing 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 ZHUSHEYE LC/MS finger printing 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
4. SHENMAI ZHUSHEYE LC/MS finger printing II mass spectrum condition
Nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Anion is selected the ion detection pattern, and cracking voltage sees Table 1 in 64 kinds of ionic m/z of selection and each the self-corresponding source.
Choose 10 batches of SHENMAI ZHUSHEYE of production in 2010, carry out SHENMAI ZHUSHEYE finger printing I and II analysis, obtain its LC/MS finger printing, be fused into a finger printing with serial mode respectively; And be standard finger-print with all batches sample average, adopt correlation coefficient process to calculate its similarity.Similarity evaluation result such as Figure 12, result show 10 batches of SHENMAI ZHUSHEYE similarities all greater than 0.9, show that quality stability is good between SHENMAI ZHUSHEYE batch.The specific implementation method of serial mode see document (Fan Xiaohui, Ye Zhengliang, Cheng Yiyu. based on the Chinese medicine multiple elements chemical finger printing similarity calculation method of information fusion, SCI. 2006,27 (1): 26-29).
SHENMAI ZHUSHEYE finger printing I and II analytical method:
1. need testing solution preparation
It is an amount of to get SHENMAI ZHUSHEYE, centrifugal 10 min of 10000 commentaries on classics/min, and it is standby to get supernatant;
2. the chromatographic condition of SHENMAI ZHUSHEYE LC/MS finger printing 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 ZHUSHEYE LC/MS finger printing 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
4. SHENMAI ZHUSHEYE LC/MS finger printing II mass spectrum condition
Nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Anion is selected the ion detection pattern, and cracking voltage sees Table 1 in 64 kinds of ionic m/z of selection and each the self-corresponding source.
Claims (4)
1. SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control, it is characterized in that, realize by following steps: the employing liquid chromatograph is a separation means, it with the mass detector two kinds of LC-MS (LC/MS) finger printing that detection means is obtained Radix Ginseng Rubra and Radix Ophiopogonis chemical compound information in the SHENMAI ZHUSHEYE of at least 10 batches of signs simultaneously, 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.
2.. a kind of SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control according to claim 1 is characterized in that concrete steps are:
(1) for the trial product formulations prepared from solutions
Get SHENMAI ZHUSHEYE more than 10 batches, carry out centrifugal 10 min of 10000 commentaries on classics/min respectively, it is standby to get supernatant;
(2) obtain finger printing I and II
With standby supernatant, by LC-MS, obtain finger printing respectively,
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 printing 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; Anion scanning detecting pattern, scanning m/z scope: 200-1400;
C. finger printing 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; Anion is selected the ion detection pattern, select the ion of 64 kinds of different m/z altogether, select ionic m/z 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 should be the separately best source of ion pair;
(3) quality stability evaluation
Get SHENMAI ZHUSHEYE finger printing I and the II more than 10 batches obtained, be fused into a finger printing with serial mode respectively, with all batches sample average is 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.
3. a kind of SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control according to claim 1 and 2, it is characterized in that, the mass spectrum condition of step (2) b finger printing 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, anion scanning detecting pattern, scanning m/z scope: 200-1400.
4. a kind of SHENMAI ZHUSHEYE mass spectrum fingerprint pattern method of quality control according to claim 1 and 2 is characterized in that, the mass spectrum condition of step (2) c finger printing II is: nitrogen temperature: 350 ℃; Atomizing pressure: 45 psi; Nitrogen flow rate: 11 L/min; Capillary voltage: 3500 V; Anion is selected the ion detection pattern, select the ion of 64 kinds of different m/z altogether, select ionic m/z 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 should be the separately best source of ion pair.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102692462A (en) * | 2012-06-03 | 2012-09-26 | 浙江大学 | Danhong injection quality control method |
| CN103728332A (en) * | 2014-01-24 | 2014-04-16 | 西南民族大学 | Finished shenmai injection liquid quality identification method |
| CN103837609A (en) * | 2012-11-26 | 2014-06-04 | 雅安三九药业有限公司 | Pulse-activating injection and preparation method thereof |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 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
- 2011-03-25 CN CN 201110073973 patent/CN102133333B/en active Active
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 (2)
| Title |
|---|
| 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》, no. 09, 20 September 2005 (2005-09-20) * |
| 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》, no. 08, 15 August 2003 (2003-08-15) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102692462A (en) * | 2012-06-03 | 2012-09-26 | 浙江大学 | Danhong injection quality control method |
| CN102692462B (en) * | 2012-06-03 | 2014-01-08 | 浙江大学 | Danhong injection quality control method |
| CN103837609A (en) * | 2012-11-26 | 2014-06-04 | 雅安三九药业有限公司 | Pulse-activating injection and preparation method thereof |
| 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 |
| CN103728332A (en) * | 2014-01-24 | 2014-04-16 | 西南民族大学 | Finished shenmai injection liquid quality identification method |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN111366672B (en) * | 2020-04-24 | 2021-06-22 | 劲牌有限公司 | Detection method of health wine fingerprint |
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| CN102133333B (en) | 2013-06-12 |
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