CN103063765A - Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection - Google Patents
Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection Download PDFInfo
- Publication number
- CN103063765A CN103063765A CN2012105624214A CN201210562421A CN103063765A CN 103063765 A CN103063765 A CN 103063765A CN 2012105624214 A CN2012105624214 A CN 2012105624214A CN 201210562421 A CN201210562421 A CN 201210562421A CN 103063765 A CN103063765 A CN 103063765A
- Authority
- CN
- China
- Prior art keywords
- ligustrazine
- ligustrazine hydrochloride
- preparation
- glucose injection
- solution
- 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.)
- Pending
Links
Images
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to ligustrazine hydrochloride, in particular to a detecting method for the ligustrazine hydrochloride in a salvia miltiorrhiza and ligustrazine glucose injection. A methanol processing detecting method is utilized in the primary standard. The methanol processing detecting method is poor in chromatographic peak pattern of the ligustrazine hydrochloride, serious in trailing, and poor in reproducibility. Meanwhile, methanol is a toxic reagent, and certain damage is brought to people and environment. Therefore, the methanol used for detecting is replaced by water. The detecting method for the ligustrazine hydrochloride is good in peak pattern, high in reproducibility, capable of reducing detecting cost, free of damage to people and environment, and particularly suitable for detecting work for the ligustrazine hydrochloride in a laboratory.
Description
Technical field:
The present invention relates to a kind of detection method of Ligustrazine Hydrochloride, refer in particular to the detection method of Ligustrazine Hydrochloride in the ginseng rhizome of chuanxiong glucose injection.
Background technology:
Ligustrazine Hydrochloride (Ligustrazine), molecular formula are C8H12N2HCl2H2O, molecular weight: 208.69, and chemical name is: 2,3,5,6-Ligustrazine, two water things, the concrete structure formula is as follows:
Ligustrazine Hydrochloride is white or off-white color crystalline powder, and smelly, bitter is arranged, and 91 ℃ of fusing points can distil.Soluble in water, be dissolved in ethanol, chloroform, the atomic benzene that is dissolved in.Ligustrazine Hydrochloride phosphate is difficult for distillation, and is comparatively stable.Effect with platelet aggregation-against, and the blood platelet of having assembled had depolymerisation; Still can expand parteriole, improve microcirculation and brain blood flow, produce the effect of antithrombotic formation and thrombus dissolving.Because phosphate is more stable, be easy to preserve, and oral also effective.
Be applicable to obliterative vascular disease, cerebral thrombosis, vasculitis, coronary heart diseases and angina pectoris etc.Acute stage, convalescence and sequelae thereof to ischemic cerebrovascular disease, such as cerebral blood supply insufficiency, cerebral thrombosis, cerebral embolism, cerebral arteriovenous malformation etc. good therapeutic effect is arranged all, can improve hemiplegia that these diseases cause, aphasia, dysphagia, extremity numbness, unable, headache, dizziness, insomnia, tinnitus, the symptoms such as shakiness, failure of memory of walking.
Summary of the invention:
Technical matters solved by the invention is to overcome the weak point in the Ligustrazine Hydrochloride detection method in the existing ginseng rhizome of chuanxiong glucose injection, provides a kind of assurance to detect accurately simultaneously, and sample peak type is good, and reappearance is good; And reduced testing cost, personnel's environment without harm, is made things convenient for the detection method of Ligustrazine Hydrochloride in the ginseng rhizome of chuanxiong glucose injection of checking.
Technical matters solved by the invention can be achieved through the following technical solutions:
The detection method of Ligustrazine Hydrochloride specifically comprises the steps: in the ginseng rhizome of chuanxiong glucose injection
1) preparation of reference substance solution
Get Ligustrazine Hydrochloride reference substance 10mg, accurately weighed, with methyl alcohol dissolving and be diluted in the 25ml measuring bottle, shake up; Precision is measured 1ml and is put in the 10ml measuring bottle again, adds methyl alcohol to scale, shakes up, in contrast product solution;
2) need testing solution preparation
The amount of taking by weighing ginseng rhizome of chuanxiong glucose injection is an amount of, adds the solution that water is made the hydrochloric ligustrazine 0.02mg of every 1ml, shakes up, and filters with the 0.45um miillpore filter, namely gets need testing solution;
Accurate reference substance solution and step 2 of measuring the step 1) preparation respectively) each 5ul of need testing solution of preparation, injecting chromatograph, the record chromatogram is pressed external standard method with calculated by peak area percentage composition and relative deviation; Wherein:
Chromatographic condition and system suitability are take 0.4% phosphoric acid: methyl alcohol mixed liquor is as mobile phase: the detection wavelength is as 292nm, 30 ℃ of column temperatures, flow velocity 1.0mi/min, chromatographic column: enlightening horse C18200*4.6; Measure according to two appendix V of Chinese Pharmacopoeia version in 2010 D regulation high performance liquid chromatography.
The present invention guarantees to detect accurately simultaneously, and sample peak type is good, and reappearance is good; And reduced testing cost, personnel's environment without harm, is conveniently checked.
Description of drawings
Fig. 1 is the collection of illustrative plates synoptic diagram of the 1# sample of test 1.
Fig. 2 is the collection of illustrative plates synoptic diagram of the 2# sample of test 1.
Fig. 3 is the collection of illustrative plates synoptic diagram of the 1# sample of test 2.
Fig. 4 is the collection of illustrative plates synoptic diagram of the 2# sample of test 2.
Embodiment
Specific embodiments of the invention given below can further be well understood to the present invention, but they are not limitation of the invention.
Concrete technical scheme is as follows:
Chromatographic condition and system suitability are take 0.4% phosphoric acid: methyl alcohol mixed liquor is as mobile phase, and the detection wavelength is 292nm, 30 ℃ of column temperatures, flow velocity 1.0mi/min, chromatographic column: enlightening horse C18200*4.6.Measure according to high performance liquid chromatography (two appendix V of Chinese Pharmacopoeia version in 2010 D).
The about 10mg of Ligustrazine Hydrochloride reference substance is got in the preparation of reference substance solution, and is accurately weighed, with methyl alcohol dissolving and be diluted in the 25ml measuring bottle, shakes up; Precision is measured 1ml and is put in the 10ml measuring bottle again, adds methyl alcohol to scale, shakes up, in contrast product solution.
Test 1:
1.1 need testing solution preparation
Taken amount ginseng rhizome of chuanxiong glucose injection is an amount of, is diluted to the solution of the hydrochloric ligustrazine 0.02mg of every 1ml with methyl alcohol, shakes up, and with miillpore filter (0.45um), filters, and get final product.
1.2 determination method is accurate each 5ul of need testing solution of measuring reference substance solution and step 1.1 preparation respectively, injecting chromatograph, and the record chromatogram is pressed external standard method with the calculated by peak area percentage composition.
Test 2:
2.1 the need testing solution preparation amount of taking by weighing ginseng rhizome of chuanxiong glucose injection is an amount of, is diluted with water to the solution of the hydrochloric ligustrazine 0.02mg of every 1ml, shakes up, and with miillpore filter (0.45um), filters, and get final product.
2.2 determination method is accurate each 5ul of need testing solution of measuring reference substance solution and step 2.1 preparation respectively, injecting chromatograph, and the record chromatogram is pressed external standard method with calculated by peak area percentage composition and relative deviation.
Test 1 and test 2 results and collection of illustrative plates contrast:
According to above-mentioned analysis of experimental data, among the present invention in the test 2 method can effectively improve the peak conditions of streaking of Ligustrazine Hydrochloride, the peak type is good, sample repeatability is high, be easy to the sample preparation avirulence, to personnel without injury, and sample detection result and test 1 indifference, and more can guarantee accuracy, the validity of testing result; Improved detection efficiency; Thereby avoid shining into the inaccurate detection error of bringing of integration because of the hangover of peak type; Reduce the use amount of organic reagent, reduced inspection cost.
Claims (1)
1. the detection method of Ligustrazine Hydrochloride in the ginseng rhizome of chuanxiong glucose injection is characterized in that, comprises the steps:
1) preparation of reference substance solution
Get Ligustrazine Hydrochloride reference substance 10mg, accurately weighed, with methyl alcohol dissolving and be diluted in the 25ml measuring bottle, shake up; Precision is measured 1ml and is put in the 10ml measuring bottle again, adds methyl alcohol to scale, shakes up, in contrast product solution;
2) need testing solution preparation
The amount of taking by weighing ginseng rhizome of chuanxiong glucose injection 1ml puts in the 50ml measuring bottle, adds water to scale, shakes up, and filters with the 0.45um miillpore filter, namely gets need testing solution;
Accurate reference substance solution and step 2 of measuring the step 1) preparation respectively) each 5ul of need testing solution of preparation, injecting chromatograph, the record chromatogram is pressed external standard method with calculated by peak area percentage composition and relative deviation; Wherein:
Chromatographic condition and system suitability are take 0.4% phosphoric acid: methyl alcohol mixed liquor is as mobile phase, and the detection wavelength is 292nm, 30 ℃ of column temperatures, flow velocity 1.0mi/min, chromatographic column: enlightening horse C18200*4.6; Measure according to two appendix V of Chinese Pharmacopoeia version in 2010 D regulation high performance liquid chromatography.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105624214A CN103063765A (en) | 2012-12-21 | 2012-12-21 | Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105624214A CN103063765A (en) | 2012-12-21 | 2012-12-21 | Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103063765A true CN103063765A (en) | 2013-04-24 |
Family
ID=48106476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105624214A Pending CN103063765A (en) | 2012-12-21 | 2012-12-21 | Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103063765A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675149A (en) * | 2013-12-19 | 2014-03-26 | 贵州景峰注射剂有限公司 | Method for detecting ligustrazine in salviae miltiorrhizae and ligusticum wallichii glucose injection |
| CN103675148A (en) * | 2013-12-19 | 2014-03-26 | 贵州景峰注射剂有限公司 | Detection method of ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine hydrochloride glucose injection |
| CN104800285A (en) * | 2015-04-24 | 2015-07-29 | 贵州景峰注射剂有限公司 | Determination method for biological activity of Shenxiong glucose injection |
-
2012
- 2012-12-21 CN CN2012105624214A patent/CN103063765A/en active Pending
Non-Patent Citations (6)
| Title |
|---|
| 何秀国等: "盐酸川芎嗪氯化钠注射液质量分析", 《中国误诊学杂志》 * |
| 叶赛银等: "高效液相色谱法测定盐酸川芎嗪的含量", 《海峡药学》 * |
| 敬永升等: "高效液相色谱法测定盐酸川芎嗪注射液的含量", 《河南大学学报（医学版）》 * |
| 李小燕: "RP-HPLC法测定盐酸川芎嗪注射液的含量", 《广西医学》 * |
| 郑林等: "UFLC法同时测定参芎葡萄糖注射液中6种主要成分", 《中成药》 * |
| 钱宏波等: "高效液相色谱法测定肾灵II号片中盐酸川芎嗪的含量", 《中国医院药学杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675149A (en) * | 2013-12-19 | 2014-03-26 | 贵州景峰注射剂有限公司 | Method for detecting ligustrazine in salviae miltiorrhizae and ligusticum wallichii glucose injection |
| CN103675148A (en) * | 2013-12-19 | 2014-03-26 | 贵州景峰注射剂有限公司 | Detection method of ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine hydrochloride glucose injection |
| CN104800285A (en) * | 2015-04-24 | 2015-07-29 | 贵州景峰注射剂有限公司 | Determination method for biological activity of Shenxiong glucose injection |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103852544B (en) | A kind of method that imatinib mesylate content and its limit of impurities are determined based on HPLC DAD methods | |
| CN101949899B (en) | Quantitative measurement method of ligustilide | |
| CN103926332B (en) | A kind of Ultra Performance Liquid Chromatography method of uridine, guanosine and adenosine content in Simultaneously test pinellia tuber extract | |
| CN103063765A (en) | Detecting method for ligustrazine hydrochloride in salvia miltiorrhiza and ligustrazine glucose injection | |
| CN104297357A (en) | Method for determining content of mythyl p-hydroxybenzoate and sodium benzoate in solution | |
| Arous et al. | Development and validation of a liquid chromatography method for the analysis of rivaroxaban and determination of its production related impurities | |
| CN101685085A (en) | Method for analyzing high performance liquid chromatography of methanesulfonic amine ginkgolide B | |
| CN103336067B (en) | High-performance liquid detection method for detecting tenofovir diethyl ester content | |
| CN102507831B (en) | Determination method of 1-deoxynojirimycin content in silkworm powder | |
| CN103792302B (en) | Method for detecting phadodendrol in cosmetics | |
| CN104950047A (en) | Method for detecting content, dissolution rate and releasing rate of memantine hydrochloride or analogues thereof in medicinal agent | |
| CN103575835B (en) | Method for determining 2-furfural in dextran-40 sodium chloride injection | |
| CN102579961B (en) | Detection method for aristolochic acid A in swelling-reducing and pain-alleviating tincture | |
| CN102928521A (en) | Method for determining contents of carbohydrate components in compound Salvia miltiorrhiza extract | |
| CN104991002A (en) | Method for quickly detecting six ingredients of dogwood by use of UFLC | |
| CN102109501B (en) | Method for detecting related substances in quinapril hydrochloride and hydrochlorothiazide composition | |
| CN104965031B (en) | Content measuring method for compound ketoprofen and omeprazole sustained-release capsules | |
| CN114778711A (en) | Method for analyzing related substances of sulfadoxine | |
| CN104374861B (en) | The method of the related substance of the western croak bulk drug of a kind of HPLC separation determination Leo | |
| CN107402277A (en) | The method of quality control of compound balloonflower root ephedrine syrup | |
| CN103513000A (en) | Method for carrying out identification and content measurement on nymphaea candida presl | |
| CN102636582A (en) | Method for determining content of diminazene and antipyrine in diminazene particle | |
| CN103063794A (en) | Content detecting and control method of epalrestat tablets | |
| CN106153756A (en) | A kind of detect the high performance liquid chromatography of rapamycin in everolimus | |
| CN105628807B (en) | A kind of quality determining method of the amino piperidines of 1 Boc 4 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130424 |