CN107064376B - A kind of method of pseudomorphine content in detection opium tincture - Google Patents
A kind of method of pseudomorphine content in detection opium tincture Download PDFInfo
- Publication number
- CN107064376B CN107064376B CN201611204081.2A CN201611204081A CN107064376B CN 107064376 B CN107064376 B CN 107064376B CN 201611204081 A CN201611204081 A CN 201611204081A CN 107064376 B CN107064376 B CN 107064376B
- Authority
- CN
- China
- Prior art keywords
- solution
- pseudomorphine
- methanol
- acid sodium
- sulfonic acid
- 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.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Quality & Reliability (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A method of applied to pseudomorphine content in opium tincture is detected in analysis field, which includes the following steps: chromatographic condition: chromatographic column: octadecylsilane chemically bonded silica is the C18 column of filler, 5 μm of partial size；Column temperature: 30 DEG C~40 DEG C；Flow velocity: 1.3ml/min~1.7ml/min；Detection wavelength: 230nm；Sample volume: 10 μ of μ l~25 l；Mobile phase: heptane sulfonic acid sodium salt and methanol；The invention is detected using HPLC method, has the advantages that reagent is easy to get, instrument uses extensive, easy to operate, testing cost is low etc. by this method detection.
Description
Technical field
The present invention relates to the methods of pseudomorphine content in one of Pharmaceutical Analysis field detection opium tincture.
Background technique
Opium tincture, the entitled Opium Tincture of English, the product are brown liquid, can play volume foam with water shaking.
It is even to be used for diarrhea, antibechic suitable for various acute intense pains.Its main composition is morphine, and morphine is in illumination, oxidation, again
It can produce the pseudomorphine being more toxic under metal ion and alkaline condition, therefore, develop pseudomorphine in a kind of opium tincture
The detection method of content is always new issue urgently to be resolved.
Summary of the invention
The purpose of the present invention is to provide a kind of detection method of pseudomorphine content in opium tincture, this method uses HPLC method
(concentration, Gradient Elution Method) is detected, and there is this method reagent to be easy to get, instrument is using extensive, easy to operate, testing cost is low
The advantages that.
The object of the present invention is achieved like this: a method of pseudomorphine content in detection opium tincture, the detection method
Include the following steps:
(1) chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica column, specification 150 × 4.6mm, 5 μm
Column temperature: 30 DEG C~40 DEG C
Flow velocity: 1.3ml/min~1.7ml/min
UV detector wavelength: 230nm
Sample volume: 10 μ of μ l~25 l
Mobile phase: heptane sulfonic acid sodium salt and methanol
(2) preparation of sodium heptanesulfonate:
Sodium heptanesulfonate 1.1g is taken, adds water 1000ml to dissolve, with 50% phosphoric acid solution tune pH to 2.6 ± 0.1；
(3) preparation of test solution:
Precision measures opium tincture 25ml, sets in 100ml measuring bottle, is diluted to scale with 1% acetum, shakes up, as confession
Test sample solution；
(4) preparation of contrast solution:
Precision measures test solution 1ml, sets in 100ml measuring bottle, adds 1% acetum to be diluted to scale, shake up；It is accurate
2ml is measured, is set in 10ml measuring bottle, is diluted to scale with 1% acetum, shakes up as contrast solution；
(5) prepared by system suitability solution
It takes morphine hydrochloride reference substance appropriate, is dissolved in water, the solution in every 1ml containing 0.2mg is made, measure 5ml, add
0.4% liquor ferri trichloridi 1ml sets in boiling water bath and heats 10 minutes, lets cool, as system suitability solution；
(6) measuring method:
Precision measures 10 μ of μ l~25 l of system suitability solution and injects liquid chromatograph, records chromatogram, the reservation of morphine
Time is 12-17 minutes, and the relative retention time of pseudomorphine is 1.7~2.0, and the separating degree between each chromatographic peak should be greater than
1.5；It is accurate respectively to measure contrast solution and 10 μ of μ l~25 l of test solution injection liquid chromatograph, chromatogram is recorded, is calculated
The content of pseudomorphine；
(7) calculation formula
In formula:
AIt is right: contrast solution main peak area；
APseudomorphine: pseudomorphine peak area in test solution；
fPseudomorphine: pseudomorphine correction factor, 0.25.
Mobile phase heptane sulfonic acid sodium salt and methanol are using concentration, Gradient Elution Method in the measuring method: the concentration,
Gradient Elution Method is following steps, and elution starts 0-2 minutes latter, heptane sulfonic acid sodium salt 85%, methanol 15%；After elution starts
2-38 minutes, heptane sulfonic acid sodium salt was by 85% to 50%, and methanol is by 15% to 50%；Elution starts 38-39 minutes latter, heptane
Sodium sulfonate solution is by 50% to 20%, and methanol is by 20% to 80%；Elution starts 39-53 minutes latter, heptane sulfonic acid sodium salt
20%, methanol 80%；Elution start it is 53-54 minutes latter, heptane sulfonic acid sodium salt by 20% to 85%, methanol by 80% to
15%；Elution starts 54-66 minutes latter, heptane sulfonic acid sodium salt 85%, methanol 15%.
The octadecylsilane chemically bonded silica column is selected from Agilent Eclipse XDB-C18 column.
The detection method of the invention for being characterized by it is detected using HPLC (concentration, Gradient Elution Method).
The detection method of pseudomorphine content compared with prior art, there is reagent to be easy to get, instrument uses in a kind of opium tincture
Extensively, the easy to operate, advantages such as testing cost is low, will be widely used in Pharmaceutical Analysis field.
Detailed description of the invention
The following describes the present invention in detail with reference to the accompanying drawings and embodiments.
Fig. 1 is system suitability Solution H PLC map of the invention.
Fig. 2 is test solution HPLC map of the invention.
Fig. 3 is contrast solution HPLC map of the invention.
Specific embodiment
Following instance will be helpful to understanding of the invention, but these examples are only for being illustrated the present invention, this hair
It is bright to be not limited to these contents.
Embodiment one
1. chromatographic condition
Chromatographic column: 5 μm of 150 × 4.6mm of Agilent (Agilent) Eclipse XDB-C18, column temperature: 30 DEG C~40 DEG C,
Flow velocity: 1.3ml/min~1.7ml/min, Detection wavelength: 230nm, sample volume: 10 μ of μ l~25 l.
2. prepared by solution
2.1 mobile phases: heptane sulfonic acid sodium salt and methanol
2.2 heptane sulfonic acid sodium salts: taking sodium heptanesulfonate 1.1g, adds water 1000ml to dissolve, with 50% phosphoric acid solution tune pH
To 2.6 ± 0.1.
2.3 test solutions: precision measures opium tincture 25ml, sets in 100ml measuring bottle, is diluted to quarter with 1% acetum
Degree, shakes up, as test solution.
2.4 contrast solutions: precision measures test solution 1ml, sets in 100ml measuring bottle, 1% acetum is added to be diluted to quarter
Degree, shakes up；Precision measures 2ml, sets in 10ml measuring bottle, is diluted to scale with 1% acetum, shakes up as contrast solution.
2.5 system suitability solution: weighing morphine hydrochloride reference substance 20.69mg, set in 100ml measuring bottle, simultaneously with water dissolution
It is diluted to scale, is shaken up；5ml is measured, adds 0.4% liquor ferri trichloridi 1ml, sets in boiling water bath and heat 10 minutes, let cool, is made
For system suitability solution.
3. measuring method
Using mobile phase heptane sulfonic acid sodium salt and methanol concentration, Gradient Elution Method；
Elution starts 0-2 minutes latter, heptane sulfonic acid sodium salt 85%, methanol 15%；Elution starts 2-38 minutes latter, heptane
Sodium sulfonate solution 85% → 50%, methanol 15% → 50%；Elution start it is 38-39 minutes latter, heptane sulfonic acid sodium salt 50% →
20%, methanol 20% → 80%；Elution starts 39-53 minutes latter, heptane sulfonic acid sodium salt 20%, methanol 80%；Elution starts
53-54 minutes afterwards, heptane sulfonic acid sodium salt 20% → 85%, methanol 80% → 15%；Elution starts 54-66 minutes latter, heptane
Sodium sulfonate solution 85%, methanol 15%.
3.1 system suitability
System suitability solution is taken, liquid chromatograph is injected；
The retention time of morphine is 15.058 minutes, and the relative retention time of pseudomorphine is 1.8, point between each chromatographic peak
It should be greater than 2.0 from degree.
The measurement of 3.2 test samples
It takes test solution to inject liquid chromatograph, records map.
3.3 blank determination
It takes contrast solution to inject liquid chromatograph, records map.
4. calculated result
In formula:
AIt is right: contrast solution main peak area；
APseudomorphine: pseudomorphine peak area in test solution；
fPseudomorphine: pseudomorphine correction factor, 0.25.
Test sample 1:
Test sample 2:
Test sample 3:
The selection of two flowing phase pH value of embodiment
Other conditions are as in the first embodiment, using heptane sulfonic acid sodium salt and methanol nitrile as mobile phase.Sodium heptanesulfonate is molten
Liquid: taking sodium heptanesulfonate 1.1g, adds water 1000ml to dissolve, with 50% phosphoric acid solution tune pH to 2.4.
The chromatographic peak of pseudomorphine is interfered by other impurities peak in test solution, can not be detected.
The selection of three mobile phase of embodiment
Other conditions are as in the first embodiment, using mobile phase heptane sulfonic acid sodium salt and acetonitrile concentration, Gradient Elution Method；
Elution starts 0-2 minutes latter, heptane sulfonic acid sodium salt 85%, acetonitrile 15%；Elution starts 2-38 minutes latter, heptane
Sodium sulfonate solution 85% → 50%, acetonitrile 15% → 50%；Elution start it is 38-39 minutes latter, heptane sulfonic acid sodium salt 50% →
20%, acetonitrile 20% → 80%；Elution starts 39-53 minutes latter, heptane sulfonic acid sodium salt 20%, acetonitrile 80%；Elution starts
53-54 minutes afterwards, heptane sulfonic acid sodium salt 20% → 85%, acetonitrile 80% → 15%；Elution starts 54-66 minutes latter, heptane
Sodium sulfonate solution 85%, acetonitrile 15%.
The chromatographic peak of pseudomorphine is interfered by other impurities peak in test solution, can not be detected.
Claims (2)
1. a kind of method of pseudomorphine content in detection opium tincture, it is characterised in that: the detection method includes the following steps:
(1) chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica column, specification 150 × 4.6mm, 5 μm
Column temperature: 30 DEG C~40 DEG C
Flow velocity: 1.3ml/min~1.7ml/min
UV detector wavelength: 230nm
Sample volume: 10 μ of μ l~25 l
Mobile phase: heptane sulfonic acid sodium salt and methanol
(2) preparation of sodium heptanesulfonate:
Sodium heptanesulfonate 1.1g is taken, adds water 1000ml to dissolve, with 50% phosphoric acid solution tune pH to 2.6 ± 0.1；
(3) preparation of test solution:
Precision measures opium tincture 25ml, sets in 100ml measuring bottle, is diluted to scale with 1% acetum, shakes up, as test sample
Solution；
(4) preparation of contrast solution:
Precision measures test solution 1ml, sets in 100ml measuring bottle, adds 1% acetum to be diluted to scale, shake up；Precision measures
2ml is set in 10ml measuring bottle, is diluted to scale with 1% acetum, is shaken up as contrast solution；
(5) prepared by system suitability solution
It takes morphine hydrochloride reference substance appropriate, is dissolved in water, the solution in every 1ml containing 0.2mg is made, measure 5ml, add 0.4%
Liquor ferri trichloridi 1ml sets in boiling water bath and heats 10 minutes, lets cool, as system suitability solution；
(6) measuring method:
Precision measures 10 μ of μ l~25 l of system suitability solution and injects liquid chromatograph, records chromatogram, the retention time of morphine
It is 12-17 minutes, the relative retention time of pseudomorphine is 1.7~2.0, and the separating degree between each chromatographic peak should be greater than 1.5；Point
It is inaccurate to measure contrast solution and 10 μ of μ l~25 l of test solution injection liquid chromatograph, chromatogram is recorded, pseudomorphine is calculated
Content；
(7) calculation formula
In formula:
AIt is right: contrast solution main peak area；
APseudomorphine: pseudomorphine peak area in test solution；
fPseudomorphine: pseudomorphine correction factor, 0.25；
Mobile phase heptane sulfonic acid sodium salt and methanol use concentration, Gradient Elution Method: the concentration, gradient in the measuring method
Elution method is following steps, and elution starts 0-2 minutes latter, heptane sulfonic acid sodium salt 85%, methanol 15%；Elution starts rear 2-38
Minute, heptane sulfonic acid sodium salt is by 85% to 50%, and methanol is by 15% to 50%；Elution starts 38-39 minutes latter, heptanesulfonic acid
Sodium solution is by 50% to 20%, and methanol is by 20% to 80%；Elution starts 39-53 minutes latter, heptane sulfonic acid sodium salt 20%, first
Alcohol 80%；Elution starts 53-54 minutes latter, and heptane sulfonic acid sodium salt is by 20% to 85%, and methanol is by 80% to 15%；Elution is opened
54-66 minutes after beginning, heptane sulfonic acid sodium salt 85%, methanol 15%.
2. the method for pseudomorphine content in a kind of detection opium tincture according to claim 1, it is characterised in that: described 18
Alkyl silane bonded silica gel column is selected from Agilent Eclipse XDB-C18 column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611204081.2A CN107064376B (en) | 2016-12-23 | 2016-12-23 | A kind of method of pseudomorphine content in detection opium tincture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611204081.2A CN107064376B (en) | 2016-12-23 | 2016-12-23 | A kind of method of pseudomorphine content in detection opium tincture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107064376A CN107064376A (en) | 2017-08-18 |
| CN107064376B true CN107064376B (en) | 2019-05-21 |
Family
ID=59619920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611204081.2A Active CN107064376B (en) | 2016-12-23 | 2016-12-23 | A kind of method of pseudomorphine content in detection opium tincture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107064376B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956798A (en) * | 2018-04-27 | 2018-12-07 | 青海省药品检验检测院 | A kind of morphine hydrochloride preparation content determining method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818635A (en) * | 2006-03-15 | 2006-08-16 | 首都师范大学 | THz inspection and fingerprint spectrum for 12 drugs |
| US8067243B2 (en) * | 2008-09-03 | 2011-11-29 | Oregon Medical Laboratories | Methods and systems for analyzing medication levels in a sample |
| CN102379927A (en) * | 2011-10-25 | 2012-03-21 | 海南海力制药有限公司 | Preparation methods of poppy shell extract and cough tablet |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005039381A2 (en) * | 2003-05-05 | 2005-05-06 | Drug Risk Solutions, L.L.C. | Compositions and processes for analysis of pharmacologic agents in biological samples |
| US20080206883A1 (en) * | 2007-02-26 | 2008-08-28 | Cody Laboratories, Inc. | Hplc method for separation and detection of hydromorphone and related opioid pharmacophores |
-
2016
- 2016-12-23 CN CN201611204081.2A patent/CN107064376B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818635A (en) * | 2006-03-15 | 2006-08-16 | 首都师范大学 | THz inspection and fingerprint spectrum for 12 drugs |
| US8067243B2 (en) * | 2008-09-03 | 2011-11-29 | Oregon Medical Laboratories | Methods and systems for analyzing medication levels in a sample |
| CN102379927A (en) * | 2011-10-25 | 2012-03-21 | 海南海力制药有限公司 | Preparation methods of poppy shell extract and cough tablet |
Non-Patent Citations (5)
| Title |
|---|
| DETERMINATION OF THE STABILITY OF MORPHINE TABLETS BY ION-PAIR REVERSED-PHASE LIQUID-CHROMATOGRAPHY;SALEM, II; GALAN, AC;《ANALYTICA CHIMICA ACTA》;19931115;第283卷(第1期);334-337 |
| HPLC法测定硫酸吗啡注射液含量的探讨;汪晓娟;《青海医药杂志》;19980930;第28卷(第9期);44-45 |
| ION-PAIR HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC DETERMINATION OF MORPHINE AND PSEUDOMORPHINE IN INJECTIONS;DOLEZALOVA, M;《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》;19920731;第10卷(第7期);507-514 |
| 中国药典中阿片系列品种吗啡含量测定方法的研究与建立( 三、四）;李永庆;《中国药品标准》;20040228;第5卷(第1期);18-21 |
| 中国药典中阿片系列品种吗啡含量测定方法的研究与建立;李永庆;《中国药品标准》;20031231;第4卷(第6期);9-11 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107064376A (en) | 2017-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101634648A (en) | Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry | |
| CN105092754A (en) | Method for determining sulfonate genotoxic impurity by using HPLC | |
| CN107255690A (en) | A kind of method of liquid chromatogram measuring malachite green | |
| CN104280475A (en) | Method for detecting content of amino acids and glycyl glutamine in compound amino acid (15) dipeptide (2) injection solution | |
| CN107064376B (en) | A kind of method of pseudomorphine content in detection opium tincture | |
| CN106556649A (en) | The detection method of disodium edetate in butyrate clevidipine injectable emulsion | |
| Choi et al. | Direct chiral analysis of primary amine drugs in human urine by single drop microextraction in‐line coupled to CE | |
| CN107515255A (en) | Utilize high performance liquid chromatograph measure Dapagliflozin and its method about material | |
| CN105181849A (en) | Method for measuring content of aminocaproic acid in caprolactam with high-performance liquid chromatography | |
| CN103630618A (en) | Method for determining betaine content in wolfberry | |
| CN104833744A (en) | Detection method for 4-methylimidazole in food | |
| CN101929988B (en) | Method for detecting febuxostat-associated matters by using high performance liquid chromatography | |
| CN104316618B (en) | A kind of HPLC method measures the method for Cys content | |
| CN102579961B (en) | Detection method for aristolochic acid A in swelling-reducing and pain-alleviating tincture | |
| CN103163228A (en) | Efficient liquid phase analysis method for hydroxyfasudil and preparation thereof | |
| CN103175930B (en) | A kind of HPLC analytical method measuring sodium sulphite content | |
| CN107703225A (en) | A kind of detection method for determining organic solvent residual in bromhexine hydrochloride raw material | |
| Martinovic-Bevanda et al. | Spectrophotometric sequential injection determination of D-penicillamine based on a complexation reaction with nickel ion | |
| CN104792888B (en) | Compound terramycin injection content determination method | |
| CN103454355A (en) | Method for analyzing and detecting content of monomer in polyacrylic resin latex solution (enteric type) product | |
| CN105158349B (en) | F in high temperature ashing ion chromatography tealeaves‑Content | |
| CN109387586B (en) | Method for measuring content of sodium cyanamide | |
| CN104897818A (en) | UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide | |
| CN105911169B (en) | Method for detecting saccharin sodium and dehydroacetic acid by high performance liquid chromatography | |
| CN111208247A (en) | Method for measuring content of gamma-hydroxybutyric acid in human hair by online heat-assisted methylation-gas chromatography mass spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |