CN104698021A - Method for detecting content of primary metabolic components in astragalus injection - Google Patents
Method for detecting content of primary metabolic components in astragalus injection Download PDFInfo
- Publication number
- CN104698021A CN104698021A CN201510031725.1A CN201510031725A CN104698021A CN 104698021 A CN104698021 A CN 104698021A CN 201510031725 A CN201510031725 A CN 201510031725A CN 104698021 A CN104698021 A CN 104698021A
- Authority
- CN
- China
- Prior art keywords
- astragalus injection
- tsp
- nmr
- peak
- kinds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for detecting the content of primary metabolic components in astragalus injection. Based on a quantitative nuclear magnetic resonance technique and a global spectral deconvolution (GSD) processing method, the content of multiple primary metabolic components in the astragalus injection is determined simultaneously, and the method particularly comprises the following steps: (1) preparing a sample solution of the astragalus injection; (2) determining a 1H-NMR fingerprint spectrum; (3) qualitatively authenticating a proton signal peak; (4) determining the content of multiple 1H-NMR components; and (5) processing the 1H-NMR spectrum and setting GSD parameters. The method has the characteristics of simplicity, convenience, feasibility, high precision, good reproducibility, high specificity and the like, and has a wide application prospect in the aspect of comprehensively detecting the quality of the astragalus injection.
Description
Technical field
The present invention relates to a kind of medicament contg detection method, especially a kind of detection method of content of astragalus injection.
Background technology
Astragalus injection is the Chinese medicine preparation developed in recent years, there is Yiqiyangyuan, strengthening vital QI to eliminate pathogenic factors, nourish heart promote blood circulation, the merit of invigorating spleen to remove dampness, be mainly used in treating that the motive is deficient, the hepatitis of the vital myocarditis of blood vessels phlegm, cardiac insufficiency and water retention due to hypofunction of the spleen.This product is as clinical commonly used drug, and domestic have tens manufacturers to produce at present.In Chinese Pharmacopoeia and ministerial standard, the quantitative target composition of Milkvetch Root and astragalus injection is Astragaloside IV, the method choice high performance liquid chromatography (HPLC) of effective constituent in traditional detection astragalus injection, although the method has many advantages, but still in following defect: 1, chromatographic resolution loss: conventional ODS chromatographic column loses the larger water soluble ingredient of polarity in detachment process; 2, common detector is lacked: certain class or a few class chemical composition can only be detected under same spectrogram; 3, standard items difficulty is separated: not easily obtain, the difficulty that qualification and quantitative test for composition bring, also improve commercial production cost simultaneously.
Quantitative proton nuclear magnetic resonance (quantitative proton nuclear magnetic resonance, q
1h-NMR) technology is a kind of increasingly mature instrument analytical method, is now widely used in chemistry, food, agricultural and military field, can be used for the purity detecting of standard substance, also can be used for the assay of various composition in potpourri.Q
1h-NMR is used for the quantitative information that the sharpest edges of Pharmaceutical Analysis are qualitative information and the assay that can simultaneously provide compound structure to confirm.Compared with HPLC method, the method without the need to determinand reference substance, sample pretreatment step is simple, specificity is strong, test speed destroys the advantages such as sample soon, not.Q
1it is absolute quantitation method that H-NMR commonly uses quantivative approach, namely makes mixed solution Simultaneously test collection of illustrative plates, by the content of the ratio determination determinand of the two peak area with the known internal standard compound of content and determinand.When carrying out quantitative test to the composition in potpourri, its key is the selection at quantitative peak, selects the assay completely independent in each composition, glitch-free characteristic signal peak just can be used for this compound.To
1h-NMR fingerprint pattern technology introduces the difficult problem faced in the chemical composition sign of traditional Chinese medicine injection:
1the chemical displacement value scope of H-NMR collection of illustrative plates is usually narrow (0-12ppm), seriously overlapped at this interval inner proton signal peak, not easily searches out completely independently that signal peak is quantitative for compound.Deconvolution (Global Spectral Deconvolution, GSD) is a kind of emerging
1h-NMR figure spectrum processing method, by the accurate correction to the deconvolution of full spectrum, accurately differentiates complicated peak shape, for overlapped signal is integrated at complicated peak each in spectrogram, isolates overlapping signal peak, and provides complete peak value and coupling constant J.The advantage of deconvolution disposal route is
1h-NMR spectrum is having the situation that impurity peaks, signal overlap and signal to noise ratio (S/N ratio) are not high, still can use the concentration of integral area deterministic compound.
Relevant astragalus injection is reported in CN104181186A patented claim disclosed in 3 days September in 2014
1the construction method of H-NMR finger-print, 25 kinds of compositions only in qualitative description astragalus injection, but fail to illustrate to the quantitative test of each composition.But the assay of characteristic chemical constituent is the important component part of traditional Chinese medicine injection quality control.Therefore, for the characteristic chemical constituent in astragalus injection, especially nascent metabolic product, find one efficiently, accurately quantivative approach there is very important using value.The present invention uses
1h-NMR collection of illustrative plates characterizes the nascent metabolic product in astragalus injection, comprises amino acid, organic acid and saccharide compound; The quantitative peak of proton signal of application deconvolution method extracting characteristic chemical constituent; Set up content assaying method and the methodological study program of multi-target ingredient; Application the method measures different manufacturers different batches astragalus injection sample
1h-NMR composes, the content difference of comparative feature composition.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of astragalus injection to come into being the detection method of content of Metabolite.
For solving the problems of the technologies described above, technical scheme of the present invention is:
Astragalus injection is come into being the detection method of content of Metabolite, based on deconvolution (GSD) quantitatively nuclear magnetic resonance technique assay is carried out to the traditional Chinese medicine ingredients of astragalus injection, concrete steps are:
(1) preparation of astragalus injection sample solution
Precision after the freeze-drying of astragalus injection sample is taken 10mg, adds 0.6ml heavy water (D
2o, containing interior mark TSP 0.2078mg/ml), be transferred in 5mm nuclear magnetic tube, seal up and be directly used in
1h-NMR tests;
(2)
1the mensuration of H-NMR finger-print
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, employing Water suppression pulse train mensuration astragalus injection sample solution
1h-NMR finger-print and reference substance solution
1h-NMR collection of illustrative plates, wherein test parameter and condition are: press down water peak sequence zgcppr, observing frequency 600.23MHz, measure temperature 298K, spectrum width 7211.5Hz, 90 ° of pulse width 13.8700 μ s, sampled data points 65536, scanning times 16 times, time delay 15s, gain acceptance in 114;
(3) Qualitive test at proton signal peak
Astragalus injection liquor
1on H-NMR collection of illustrative plates, proton signal peak is distributed between δ 0-5.5, wherein δ 0.0-3.2 is amino acid and organic acid proton characteristic signal district, δ 3.3-5.5 is saccharide matrix subcharacter signaling zone, a point situation is split according to the chemical displacement value at proton signal peak and coupling, in conjunction with the two-dimensional nucleus magnetic chart spectrum information of astragalus injection, identify 20 kinds of nascent Metabolites and 4 kinds of secondary metabolism compositions altogether, be respectively
Table 1 astragalus injection is come into being Metabolite
1h-NMR belongs to
(4)
1the multicomponent assay of H-NMR
To select in compound 8 independently diagnostic protons signal peak as quantitative peak, 3-(trimethyl silyl) propionic acid-d
4sodium salt (TSP) is interior mark compound, applies the concentration that following formula to measure in astragalus injection 8 kinds of nascent Metabolite acetic acid, proline, pyroglutamic acid, malonic acid, glycocoll, glucose, sucrose, formic acid,
Wherein P
xand P
tSPbe respectively the concentration of compound and TSP, A
xand A
tSPthe integral area at the quantitative peak of compound and TSP methyl peak respectively, N
xand N
tSPthe proton number at the quantitative peak of representation compound and TSP methyl peak respectively, M
xand M
tSPthe molecular weight of compound and TSP respectively;
(5)
1the process of H-NMR spectrum is conciliate deconvolution parameter and is arranged
Adopt MetresNova software to test
1h-NMR finger-print enters horizontal phasing control, baseline correction, calibration reconciliation process of convolution successively.In deconvolution optimum configurations, the setting value of J-Tolerance is 0.4Hz, can measure the content of astragalus injection 8 kinds of nascent Metabolites according to step (4) described method.
The invention has the beneficial effects as follows:
The detection method of content of above-mentioned astragalus injection, effectively can solve the quantitative test problem of the compositions such as carbohydrate in astragalus injection, amino acids, organic acid, described method has simple and easy to do, the feature such as good stability, precision are high, favorable reproducibility, accuracy is high, specificity is strong, has broad application prospects realizing astragalus injection total quality context of detection.
Accompanying drawing explanation
Fig. 1 is 5 producer's astragalus injection sample solutions
1h-NMR finger-print, wherein, A-is honest
QINGCHUN BAO, B-Heilungkiang jewellery, C-Shijiazhuang martial prowess, D-Dali, new Asia, E-Shanghai;
Fig. 2 is astragalus injection
1the quantitative peak of 8 kind representative compositions of H-NMR finger-print by obtaining after deconvolution process;
Fig. 3 is rubble figure and the shot chart of the PCA analysis of the astragalus injection of 5 producers, wherein, and QCB: honest QINGCHUN BAO, ZB: Heilungkiang jewellery, SW: Shijiazhuang martial prowess, DL: Dali, XY: new Asia, Shanghai;
Fig. 4 is the content of 8 kinds of compositions in 5 producer's astragalus injection samples, wherein, and QCB: honest QINGCHUN BAO, ZB: Heilungkiang jewellery, SW: Shijiazhuang martial prowess, DL: Dali, XY: new Asia, Shanghai.
Embodiment
In order to make those skilled in the art better understand technical scheme of the present invention, below in conjunction with embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
Astragalus injection
1the foundation of H-NMR standard finger-print
1.1 instruments and reagent
BRUKER AVANCE III 600 type NMR spectrometer with superconducting magnet, proton excitation frequency 600.23MHz, configuration BBFO positive observes broadband probe and BVT3200 numeral temperature controller, 5mm standard nuclear-magnetism sample hose, NORELL company of the U.S. produces, D
2o deuterated degree >99.8%, Sigma-Aldrich, deuterated degree >98%, the Sigma-Aldrich company of 3-(trimethyl silyl) propionic acid-d4 sodium salt (TSP) produces, experiment astragalus injection is commercially available prod, specification is for often propping up dress 10ml, there is the astragalus injection that 5 producers have 20 batches altogether, be respectively honest QINGCHUN BAO medicine company (1311102), Heilungkiang jewellery medicine company (A20120709, A20130206), Shijiazhuang martial prowess medicine company (131001D2, 130324D1, 130803D2, 130525D2, 131116D3, 130326D1, 130313D2), Dali medicine company (1301072, 1307222, 1309212), new Asia, Shanghai medicine company (130402-3, 131002-2, 130401-1, 131003-1, 131010-3, 130508-1, 131007-2).
The preparation of 1.2 astragalus injection test sample solution
Get astragalus injection sample quick freeze in-80 DEG C of refrigerators, then to put it in vacuum freezing drying oven precision after freeze-drying and take 10mg, add 0.6ml D
2o (containing interior mark TSP 0.02g/ml), is transferred in 5mm nuclear magnetic tube, seals up and be directly used in
1h-NMR tests.
1.3
1the mensuration of H-NMR finger-print
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, employing Water suppression pulse train zgcppr mensuration astragalus injection sample solution
1h-NMR finger-print.Observing frequency 600.23MHz, measure temperature 298K, spectrum width 12019.2Hz, 90 ° of pulse width 13 μ s, sampled data points 65536, scanning times 16 times, time delay 15s, gain acceptance in 128.
1.4
1the qualification at H-NMR finger-print proton signal peak
1h-NMR finger-print is through phase correction, after baseline correction and chemical shift correct, a point situation is split according to the chemical displacement value at proton signal peak and coupling, two-dimensional nucleus magnetic chart spectrum information in conjunction with astragalus injection control sample identifies leucine, lactic acid, ethanol, threonine, alanine, arginine, acetic acid, proline, pyroglutamic acid, succinic acid, malonic acid, glucose, betaine, sweet mellow wine, sucrose, fructose, glycocoll, melitriose, arabinose, calycosin, calycosin-7-O-β-D-glucopyranose, formic acid, onocerin, 2 '-hydroxyl-3 ', 4 '-dimethyl isoflavan-7-O-β-D-glucopyranose, totally 24 kinds of compositions (Fig. 1), comprising the characteristic chemical constituent of the Radix Astragali, amino acid, organic acid and carbohydrate content, detailed chemical shift ownership is in table 1.Select 8 kinds of representational nascent Metabolites, application deconvolution disposal route extracts the quantitative peak (Fig. 2) of each composition, carries out assay analysis.
1.5 methodological study
Apply the quantitative peak of 8 kinds of nascent Metabolites in common integration method and deconvolution method extraction sample respectively, in deconvolution optimum configurations, the setting value of J-Tolerance is 0.4Hz.Linear, stability, precision, repeatability and the average recovery of two kinds of disposal routes are investigated.
Precision: get with a astragalus injection need testing solution, above-mentioned
1measure finger-print continuous 6 times under H-NMR test condition, record quantitative peak integral area, calculate RSD value.
Repeatability: get same batch of astragalus injection need testing solution 6 parts, test
1h-NMR finger-print, records quantitative peak integral area, calculates RSD value.
Stability test: get with a astragalus injection need testing solution, respectively at 0,2,4,6,8,12,24h, test
1h-NMR collection of illustrative plates, records quantitative peak integral area, calculates RSD value.
Linear: precision takes standard items, put with 2mL volumetric flask, be diluted to scale with the heavy water containing TSP, shake up, doubling dilution obtains the titer of 5 variable concentrations, respectively gets 0.6ml and is placed in nuclear magnetic tube, measures
1h-NMR collection of illustrative plates, records the integral area at the quantitative peak of each standard items, calculates typical curve.
Average recovery: precision takes astragalus injection test sample 5mg, totally 6 parts, then precision adds 8 kinds of standard items potpourri 5mg respectively, acetic acid, proline, pyroglutamic acid, alanine, glycocoll, glucose, sucrose, formic acid are diluted to concentration and are respectively 0.08960mg/ml, 0.9858mg/ml, 0.4674mg/ml, 0.2693mg/ml, 0.4579mg/ml, 0.3551mg/ml, 0.0870mg/ml, 0.0289mg/ml, measure
1h-NMR collection of illustrative plates, record integral area, calculates the recovery.
The acetic acid under common integration, proline, pyroglutamic acid, malonic acid, glycocoll, glucose, sucrose, formic acid 8 kinds of linear R of nascent Metabolite can be drawn by table 2
2for 0.9763-0.9990, precision RSD value scope 1.62%-4.65%, stability RSD value scope 0.75%-8.59%, repeated RSD value scope 0.94%-4.57%, the scope 80.69%-98.08% of average recovery; Table 3 is the lower 8 kinds of linear R of nascent Metabolite of deconvolution disposal route
2for 0.999-0.9998, precision RSD value scope 1.98%-3.79%, stability RSD value scope 0.41%-4.50%, repeated RSD value scope 1.37%-2.66%, the scope 91.40%-102.69% of average recovery.
Linear, precision, stability, the repeatability of experimental result (table 2 and table 3) Explicit solutions convolution quantitative nuclear-magnetism method are totally better than the quantitative nuclear-magnetism method of common integration.
The common integration of table 2 quantitative nuclear-magnetism method methodological study
Table 3 deconvolution quantitative nuclear-magnetism method methodological study
1.6 deconvolution quantitative nuclear-magnetism method measures the content of 8 kinds of nascent metabolic products in different manufacturers astragalus injection
Adopt deconvolution
18 kinds of nascent metabolic products in the astragalus injection of H-NMR determination of quantitative analysis 5 producers 20 batches: the content of acetic acid, proline, pyroglutamic acid, malonic acid, glycocoll, glucose, sucrose, formic acid.Result is see table 4.
The assay of table 4 20 batches of astragalus injection samples
1.7 pattern recognition analysis
5 kinds of producer (QCB: honest QINGCHUN BAO; ZB: Heilungkiang jewellery; SW: Shijiazhuang martial prowess; DL: Dali; XY: new Asia, Shanghai) the NMR data (each batch of number n=3) of 20 batches of astragalus injection samples, 60 samples altogether, principal component analysis (PCA) (principal components analysis, PCA) method is adopted to carry out cluster analysis to different manufacturers astragalus injection.Rubble figure (Fig. 3 A) display that PCA analyzes: the first two major component (PC1 and PC2) accumulation explanatory variable is more than 90%; Shot chart (Fig. 3 B) display of PCA: 5 producer's astragalus injection samples have effect of significantly dividing into groups, and each producer is distinguished separately, between prompting different manufacturers, the content difference of 8 kinds of nascent Metabolites is comparatively large, has statistical significance.
The contents level that box traction substation (Fig. 4) also show acetic acid, proline, pyroglutamic acid, malonic acid, glycocoll, glucose, sucrose, formic acid 8 kinds of representative compositions in 5 kinds of producer's astragalus injection samples differs greatly, and experimental result prompting amino acid, organic acid, saccharide compound have important impact to the astragalus injection distinguishing different manufacturers.
Visible, principle of the present invention sets up one based on the quantitative nuclear magnetic resonance technique of deconvolution, applies to traditional Chinese medicine ingredients assay, present invention is specifically related to astragalus injection, astragalus injection
1h-NMR finger-print, a collection of illustrative plates completes the qualitative and quantitative analysis of nascent Metabolite in astragalus injection simultaneously, also compensate for the defect that conventional HPLC finger-print can't detect mentioned component simultaneously.
Above-mentioned detailed description of the detection method of content that this kind of astragalus injection comes into being Metabolite being carried out with reference to embodiment; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Claims (2)
1. the detection method of content of nascent Metabolite in astragalus injection, is characterized in that: conciliate convolution processing method based on quantitative nuclear magnetic resonance technique and carry out assay to the Multiple components in astragalus injection simultaneously, concrete steps are:
(1) preparation of astragalus injection sample solution
Precision after the freeze-drying of astragalus injection sample is taken 10mg, adds the D of 0.6ml containing interior mark TSP0.2078mg/ml
2o, is transferred in 5mm nuclear magnetic tube, seals up and be directly used in
1h-NMR tests;
(2)
1the mensuration of H-NMR finger-print
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, employing Water suppression pulse train mensuration astragalus injection sample solution
1h-NMR finger-print and reference substance solution
1h-NMR collection of illustrative plates, wherein test parameter and condition are: press down water peak sequence zgcppr, observing frequency 600.23MHz, measure temperature 298K, spectrum width 7211.5Hz, 90 ° of pulse width 13.8700 μ s, sampled data points 65536, scanning times 16 times, time delay 15s, gain acceptance in 114;
(3) Qualitive test at proton signal peak
Astragalus injection liquor
1on H-NMR collection of illustrative plates, proton signal peak is distributed between δ 0-5.5, wherein δ 0.0-3.2 is amino acid and organic acid proton characteristic signal district, δ 3.3-5.5 is saccharide matrix subcharacter signaling zone, a point situation is split according to the chemical displacement value at proton signal peak and coupling, in conjunction with the two-dimensional nucleus magnetic chart spectrum information of astragalus injection, identify 20 kinds of nascent metabolic products and 4 kinds of secondary metabolism compositions altogether;
(4)
1the multicomponent assay of H-NMR
With 3-(trimethyl silyl) propionic acid-d
4sodium salt is interior mark compound, applies the concentration that following formula to measure in astragalus injection 8 kinds of nascent Metabolite acetic acid, proline, pyroglutamic acid, malonic acid, glycocoll, glucose, sucrose, formic acid:
Wherein P
xand P
tSPbe respectively the concentration of compound and TSP, A
xand A
tSPthe integral area at the quantitative peak of compound and TSP methyl peak respectively, N
xand N
tSPthe proton number at the quantitative peak of representation compound and TSP methyl peak respectively, M
xand M
tSPthe molecular weight of compound and TSP respectively;
(5)
1the process of H-NMR spectrum is conciliate deconvolution parameter and is arranged
To adopt MetresNova software to obtaining
1h-NMR finger-print enters horizontal phasing control, baseline correction, calibration reconciliation process of convolution successively, in deconvolution optimum configurations, the setting value of J-Tolerance is 0.4Hz, can measure the content of astragalus injection 8 kinds of nascent Metabolites according to step (4) described method.
2. the detection method of content of nascent Metabolite in astragalus injection according to claim 1, is characterized in that: 20 kinds of nascent Metabolites and 4 kinds of secondary metabolism compositions in described step (3), be respectively:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510031725.1A CN104698021B (en) | 2015-01-22 | 2015-01-22 | Method for detecting content of primary metabolic components in astragalus injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510031725.1A CN104698021B (en) | 2015-01-22 | 2015-01-22 | Method for detecting content of primary metabolic components in astragalus injection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104698021A true CN104698021A (en) | 2015-06-10 |
| CN104698021B CN104698021B (en) | 2017-01-18 |
Family
ID=53345370
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510031725.1A Expired - Fee Related CN104698021B (en) | 2015-01-22 | 2015-01-22 | Method for detecting content of primary metabolic components in astragalus injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104698021B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954311A (en) * | 2016-06-22 | 2016-09-21 | 四川好医生攀西药业有限责任公司 | Method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and extract of Periplaneta americana |
| CN107064199A (en) * | 2017-01-23 | 2017-08-18 | 贵州大学 | A kind of trans cucurbit(7)uril recognizes the application of biogenic amine |
| CN109596660A (en) * | 2019-01-07 | 2019-04-09 | 山西大学 | A kind of discrimination method of Qinzhou Huang millet |
| CN109696449A (en) * | 2018-12-13 | 2019-04-30 | 北京市食品安全监控和风险评估中心（北京市食品检验所） | The method for detecting a variety of small molecule water soluble substances in milk powder product simultaneously |
| CN110208447A (en) * | 2019-07-02 | 2019-09-06 | 山西大学 | The construction method of compound flavescent sophora root injection 1H-NMR finger-print and application |
| CN112525943A (en) * | 2020-11-19 | 2021-03-19 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | By using q1Method for quantitatively analyzing ethanol and acetic acid in fermented fruit and vegetable juice by H-NMR technology |
| CN113030291A (en) * | 2021-01-28 | 2021-06-25 | 成都第一制药有限公司 | HPLC-ELSD characteristic spectrum of motherwort injection and establishing method thereof |
| CN113024419A (en) * | 2021-02-01 | 2021-06-25 | 天津中医药大学 | Extraction and detection method of trimethylamine oxide and betaine |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2049192A (en) * | 1979-02-21 | 1980-12-17 | Nicolet Instrument Corp | Temperature measurement in nuclear magnetic resonance spectrometry |
| US20050208138A1 (en) * | 2000-12-18 | 2005-09-22 | Yang David J | Local regional chemotherapy and radiotherapy using in situ hydrogel |
| US20100099633A1 (en) * | 2005-06-23 | 2010-04-22 | Nuliv Holding Inc. | Method for enhancing nutrient absorption with astragalosides |
| CN103884731A (en) * | 2013-12-28 | 2014-06-25 | 丽珠集团利民制药厂 | Nuclear magnetic resonance quality control method for ginseng and astragalus strengthening injection |
| CN104181186A (en) * | 2014-09-03 | 2014-12-03 | 山西大学 | Construction method of <1>H-NMR fingerprint of radix astragali injection |
-
2015
- 2015-01-22 CN CN201510031725.1A patent/CN104698021B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2049192A (en) * | 1979-02-21 | 1980-12-17 | Nicolet Instrument Corp | Temperature measurement in nuclear magnetic resonance spectrometry |
| US20050208138A1 (en) * | 2000-12-18 | 2005-09-22 | Yang David J | Local regional chemotherapy and radiotherapy using in situ hydrogel |
| US20100099633A1 (en) * | 2005-06-23 | 2010-04-22 | Nuliv Holding Inc. | Method for enhancing nutrient absorption with astragalosides |
| CN103884731A (en) * | 2013-12-28 | 2014-06-25 | 丽珠集团利民制药厂 | Nuclear magnetic resonance quality control method for ginseng and astragalus strengthening injection |
| CN104181186A (en) * | 2014-09-03 | 2014-12-03 | 山西大学 | Construction method of <1>H-NMR fingerprint of radix astragali injection |
Non-Patent Citations (2)
| Title |
|---|
| 林珊 等: "定量核磁共振技术在中药分析中的应用进展", 《药学实践杂志》 * |
| 陈燕燕等: "应用核磁共振指纹谱考察黄芪不同炮制品", 《中国科技论文》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954311A (en) * | 2016-06-22 | 2016-09-21 | 四川好医生攀西药业有限责任公司 | Method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and extract of Periplaneta americana |
| CN107064199A (en) * | 2017-01-23 | 2017-08-18 | 贵州大学 | A kind of trans cucurbit(7)uril recognizes the application of biogenic amine |
| CN109696449A (en) * | 2018-12-13 | 2019-04-30 | 北京市食品安全监控和风险评估中心（北京市食品检验所） | The method for detecting a variety of small molecule water soluble substances in milk powder product simultaneously |
| CN109596660A (en) * | 2019-01-07 | 2019-04-09 | 山西大学 | A kind of discrimination method of Qinzhou Huang millet |
| CN110208447A (en) * | 2019-07-02 | 2019-09-06 | 山西大学 | The construction method of compound flavescent sophora root injection 1H-NMR finger-print and application |
| CN112525943A (en) * | 2020-11-19 | 2021-03-19 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | By using q1Method for quantitatively analyzing ethanol and acetic acid in fermented fruit and vegetable juice by H-NMR technology |
| CN112525943B (en) * | 2020-11-19 | 2024-04-19 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | Q is adopted1Method for quantitatively analyzing ethanol and acetic acid in fermented fruit and vegetable juice by H-NMR technology |
| CN113030291A (en) * | 2021-01-28 | 2021-06-25 | 成都第一制药有限公司 | HPLC-ELSD characteristic spectrum of motherwort injection and establishing method thereof |
| CN113024419A (en) * | 2021-02-01 | 2021-06-25 | 天津中医药大学 | Extraction and detection method of trimethylamine oxide and betaine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104698021B (en) | 2017-01-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104698021A (en) | Method for detecting content of primary metabolic components in astragalus injection | |
| CN103713004B (en) | A kind of magnetic resonance detection method of Chinese medicine injection | |
| CN103884731B (en) | A kind of SHENQI FUZHENG ZHUSHEYE nuclear magnetic resonance, NMR method of quality control | |
| Zuriarrain et al. | Quantitative determination of ethanol in cider by 1H NMR spectrometry | |
| Lian et al. | Direct and simultaneous quantification of ATP, ADP and AMP by 1H and 31P Nuclear Magnetic Resonance spectroscopy | |
| Wang et al. | A series of strategies for solving the shortage of reference standards for multi-components determination of traditional Chinese medicine, Mahoniae Caulis as a case | |
| CN106814150A (en) | A kind of isotopic dilution Ultra Performance Liquid Chromatography MS vitamin K1Method | |
| Gonzalez et al. | Authentication of lemon juices and concentrates by a combined multi-isotope approach using SNIF-NMR and IRMS | |
| CN107703233A (en) | A kind of detection method of adenosine content | |
| CN106501393B (en) | A method of detection hickory chick Nucleosides | |
| CN111999332A (en) | Method for measuring content of turanose in honey by using nuclear magnetic hydrogen spectrometry | |
| Goldoni et al. | A simple and accurate protocol for absolute polar metabolite quantification in cell cultures using quantitative nuclear magnetic resonance | |
| CN110133169A (en) | A kind of method and application using frusemide in LC-MS detection human plasma | |
| CN107421975B (en) | The detection method of glycerol content in a kind of injection | |
| CN104931519A (en) | Content detection method of salvianolic acid injection liquid | |
| CN108956816A (en) | The HPLC analysis method of curcumin and 5 FU 5 fluorouracil concentration in blood plasma is measured simultaneously | |
| CN105911081B (en) | A kind of method for differentiating mannatide | |
| CN104880478A (en) | Method for detecting content of glycerophosphoryl choline | |
| CN105954311A (en) | Method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and extract of Periplaneta americana | |
| CN107014853A (en) | A kind of detection method of content of sodium tashinone II A sulfonate injection | |
| CN109856267B (en) | Method for simultaneously determining contents of multiple components in Chinese medicinal preparation based on LC-MS technology | |
| CN111721794A (en) | Method for quantitatively detecting 5-hydroxymethylfurfural in yellow wine by utilizing nuclear magnetic resonance hydrogen spectrum | |
| CN106124551B (en) | Buddha's hand hydrogen nuclear magnetic resonance finger-print and its method for building up and purposes | |
| Gupta et al. | Techniques for detection and extraction of metabolites | |
| CN109828040B (en) | Construction method and detection method of UPLC (ultra Performance liquid chromatography) characteristic spectrum of eclipta medicinal material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170118 Termination date: 20220122 |