CN102565260A - Method for preparing diacetylmorphine hydrochloride standard substance - Google Patents
Method for preparing diacetylmorphine hydrochloride standard substance Download PDFInfo
- Publication number
- CN102565260A CN102565260A CN2011104285548A CN201110428554A CN102565260A CN 102565260 A CN102565260 A CN 102565260A CN 2011104285548 A CN2011104285548 A CN 2011104285548A CN 201110428554 A CN201110428554 A CN 201110428554A CN 102565260 A CN102565260 A CN 102565260A
- Authority
- CN
- China
- Prior art keywords
- diacetylmorphine
- standard substance
- hydrochloride standard
- preparation
- diacetylmorphine hydrochloride
- 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
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing a diacetylmorphine hydrochloride standard substance. The method comprises the following steps of: preparing a methanol solution of a diacetylmorphine sample, and adding ethanol to adjust the polarity of the solution; performing preparation and purification by using a middle-pressure preparation system under the chromatographic conditions that a filler of a chromatographic column is an amino-bonded silica filler, a detection wavelength is 228 nm, an auxiliary wavelength is 215 nm, a mobile phase A is chromatographic pure normal hexane and a mobile phase B is chromatographic pure ethanol; performing gradient elution; concentrating reduced pressure concentration on main peak receiving liquid, which is prepared, in a rotary evaporator at the temperature of 30 to 55 DEG C to obtain the diacetylmorphine hydrochloride standard substance; and storing the diacetylmorphine hydrochloride standard substance in nitrogen environment, and detecting the purity of the diacetylmorphine hydrochloride standard substance. By adoption of the method, exposure of diacetylmorphine in air can be reduced, so hydrolytic spoilage of the diacetylmorphine is avoided, and the diacetylmorphine hydrochloride standard substance with high purity of over 99 percent is prepared. The method has the advantages of short preparation time, simple process, low cost and safety in operation, and the chromatographic column is reusable.
Description
Technical field
The present invention relates to a kind of preparation method of diacetylmorphine hydrochloride standard substance.
Background technology
Diacetylmorphine is a kind of narcotics, and its common form is the diacetylmorphine hydrochloride.At present, China's forensic sciences at different levels laboratory qualitative, quantitative check evaluation work of mainly adopting chromatographic process to carry out to discover and seize the diacetylmorphine sample.Therefore, want to obtain accurate, reliable expert's conclusion, must use diacetylmorphine hydrochloride standard substance.In addition, have the traceability and corresponding uncertainty of measurement of science in order to ensure the analytical test result, the forensic science laboratory should adopt diacetylmorphine hydrochloride standard substance that corresponding analysis test method is confirmed before carrying out analytical test.In addition, diacetylmorphine hydrochloride standard substance in the ability of setting up breadboard quality management system, check court research laboratory and staff thereof, implement between the laboratory aspect such as value comparison, also play crucial effect.
Present stage, domestic do not have research institution that diacetylmorphine hydrochloride standard substance can be provided, and then there are problems such as costly, that formality is loaded down with trivial details, the arrival cycle is long in the external diacetylmorphine hydrochloride standard substance of producing of import.At present; The qualitative, quantitative check evaluation work of increasing diacetylmorphine sample is just being born in forensic sciences at different levels laboratory; For promote its analytical test level comprehensively; Strengthen the accuracy and the confidence level of its check probation report of providing, urgent just day by day to the demand of diacetylmorphine hydrochloride standard substance.
The present invention aims to provide a kind of economy, diacetylmorphine hydrochloride standard substance preparation method fast and effectively; Can remedy the technological deficiency of China aspect the development of diacetylmorphine hydrochloride standard substance, improve domesticly relying on external situation fully in diacetylmorphine hydrochloride standard substance supply side; Simultaneously; The present invention will solve the forensic science laboratory and carry out a difficult problem that lacks diacetylmorphine hydrochloride standard substance when the check of diacetylmorphine sample qualitative, quantitative is identified, reduce the funds spending that court of basic unit research laboratory buys diacetylmorphine hydrochloride standard substance.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the preparation method that a kind of preparation speed is fast, can effectively avoid diacetylmorphine hydrolysis and acquisition high-purity (more than 99%) diacetylmorphine hydrochloride standard substance is provided.
Technical scheme of the present invention is summarized as follows:
A kind of preparation method of diacetylmorphine hydrochloride standard substance may further comprise the steps:
A. being the diacetylmorphine sample solution of 0.5g/mL with methyl alcohol for the solvent compound concentration, is that the ratio of 1g: 1.5-2.3mL adds ethanol adjustment solution polarity in the ratio of said diacetylmorphine sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 228nm, auxiliary wavelength 215nm; Moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains diacetylmorphine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity.
The said amino of said amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups, and the specification of said filler is sphere or the indefinite form of 3-100 μ m.
Said moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, and condition of gradient elution is: B increases to 50% by volumetric concentration 15% in 40min, keeps 50% wash-out 40min then.
Characteristics of the present invention are: 1, can reduce the aerial exposure of diacetylmorphine, thereby avoid the diacetylmorphine hydrolytic spoilage, successfully prepare highly purified diacetylmorphine hydrochloride standard substance more than 99% first; 2, has the advantage that preparation time is short, chromatographic column can reuse; 3, it is low to have a simple cost of technology, the advantage of handling safety.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
Embodiment 1
A kind of preparation method of diacetylmorphine hydrochloride standard substance may further comprise the steps:
A. accurately take by weighing diacetylmorphine sample 40mg, add methyl alcohol to 80 μ l dissolving, to wherein adding 80 μ l absolute ethyl alcohols, make it to dissolve each other again with moving phase with the adjustment solution polarity;
B. the sample solution that step a is obtained injects compacting and is equipped with the systems produce purifying, and chromatographic condition is: 20-45 μ m HILIC chromatographic column (its filler is that secondary amine and tertiary amine mass ratio are 3: 2 mixed fillers), three series connection of 12g+12g+12g; Flow velocity 20ml/min; Detect wavelength 228nm, auxiliary wavelength 215nm, moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol; Gradient elution, gradient condition is following:
C. with the 32-47min place receive liquid (being that main peak receives liquid) collect the back in 50 ℃ of Rotary Evaporators ,-0.8～-0.95Mpa concentrates down and obtains diacetylmorphine hydrochloride standard substance, nitrogen environment is preserved down, adopting gas chromatograph to detect its purity is 99.58%.
Embodiment 2:
A kind of preparation method of diacetylmorphine hydrochloride standard substance may further comprise the steps:
A. accurately take by weighing diacetylmorphine sample 100mg and add methyl alcohol to 200 μ l dissolving, to wherein adding 150 μ l absolute ethyl alcohols, make it to dissolve each other again with moving phase with the adjustment solution polarity;
B. the sample solution that step a is obtained injects compacting and is equipped with the systems produce purifying; Chromatographic condition is: 10 μ m HILIC chromatographic columns (its filler is that the mass ratio of primary amine and secondary amine is 9: 1 a mixed fillers), three series connection of 20g+20g+20g; Flow velocity 30ml/min detects the auxiliary wavelength 215nm of wavelength 228nm, moving phase: A normal hexane (import chromatographically pure), B absolute ethyl alcohol (import chromatographically pure); Gradient elution, gradient condition is following:
C. with the 53.5-65min place receive liquid (being that main peak receives liquid) collect the back in 50 ℃ of Rotary Evaporators ,-0.8～-0.95Mpa concentrates down and obtains the hydrochloride standard substance, nitrogen environment is preserved down, adopts gas chromatograph to detect its purity 99.66%.
Embodiment 3:
A kind of preparation method of diacetylmorphine hydrochloride standard substance may further comprise the steps:
A. accurately take by weighing sample 4g and add methyl alcohol and dissolve to 8ml, make it to dissolve each other with the adjustment solution polarity to wherein adding the 9.2ml absolute ethyl alcohol again with moving phase;
B. the sample solution that step a is obtained injects compacting and is equipped with the systems produce purifying: 50-100 μ m HILIC chromatographic column (its filler is that the mass ratio of secondary amine and tertiary amine is 3: 2 a mixed fillers) three series connection of 80g+80g+80g; Flow velocity 55ml/min; Detect the auxiliary wavelength 215nm of wavelength 228nm; Moving phase: A normal hexane (import chromatographically pure), B absolute ethyl alcohol (import chromatographically pure), gradient elution, gradient condition is following:
C. with the 60-75min place receive liquid (being that main peak receives liquid) collect the back in 50 ℃ of Rotary Evaporators ,-0.8～-0.95Mpa concentrates down and obtains the hydrochloride standard substance, nitrogen environment is preserved down, adopts gas chromatograph to detect its purity 99.64%.
But the chromatographic column activating and regenerating, regeneration step is: with the methanol solution that contains 5% formic acid with the 30mL/min flow velocity behind post 1h, with pure water with the 30mL/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with 30mL/min respectively towards post 30min.
Claims (3)
1. the preparation method of a diacetylmorphine hydrochloride standard substance is characterized in that may further comprise the steps:
A. being the diacetylmorphine sample solution of 0.5g/mL with methyl alcohol for the solvent compound concentration, is that the ratio of 1g: 1.5-2.3mL adds ethanol adjustment solution polarity in the ratio of said diacetylmorphine sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 228nm, auxiliary wavelength 215nm; Moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains diacetylmorphine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity.
2. the preparation method of a kind of diacetylmorphine hydrochloride standard substance according to claim 1; It is characterized in that the said amino of said amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups, the specification of said filler is sphere or the indefinite form of 3-100 μ m.
3. the preparation method of a kind of diacetylmorphine hydrochloride standard substance according to claim 1; It is characterized in that said moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol; Condition of gradient elution is: B increases to 50% by volumetric concentration 15% in 40min, keeps 50% wash-out 40min then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110428554.8A CN102565260B (en) | 2011-12-20 | 2011-12-20 | Method for preparing diacetylmorphine hydrochloride standard substance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110428554.8A CN102565260B (en) | 2011-12-20 | 2011-12-20 | Method for preparing diacetylmorphine hydrochloride standard substance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102565260A true CN102565260A (en) | 2012-07-11 |
| CN102565260B CN102565260B (en) | 2014-07-30 |
Family
ID=46411221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110428554.8A Active CN102565260B (en) | 2011-12-20 | 2011-12-20 | Method for preparing diacetylmorphine hydrochloride standard substance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102565260B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749402A (en) * | 2012-08-07 | 2012-10-24 | 公安部禁毒情报技术中心 | Preparation method of morphine hydrochloride standard substance |
| CN102759476A (en) * | 2012-07-20 | 2012-10-31 | 公安部禁毒情报技术中心 | Preparation method of cocaine hydrochloride standard substance |
| CN107304213A (en) * | 2016-04-20 | 2017-10-31 | 中国医药工业有限公司 | A kind of opium poppy extract-treated method and apparatus |
| CN107345946A (en) * | 2017-05-08 | 2017-11-14 | 公安部物证鉴定中心 | Method for preparing purified for the methcathinone standard substance of forensic science illicit drugs inspection |
| CN107478733A (en) * | 2017-05-08 | 2017-12-15 | 公安部物证鉴定中心 | Method for preparing purified for the codeine standard substance of forensic science illicit drugs inspection |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999022244A2 (en) * | 1997-10-27 | 1999-05-06 | Varian, Inc. | Method for determination of drugs of abuse in biological samples |
| CN1818635A (en) * | 2006-03-15 | 2006-08-16 | 首都师范大学 | THz inspection and fingerprint spectrum for 12 drugs |
| CN101750458A (en) * | 2009-11-05 | 2010-06-23 | 香港科技大学 | Method for detecting drug residues in human body |
| CN102128905A (en) * | 2010-12-10 | 2011-07-20 | 中国广州分析测试中心 | Method for quickly detecting drug |
-
2011
- 2011-12-20 CN CN201110428554.8A patent/CN102565260B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999022244A2 (en) * | 1997-10-27 | 1999-05-06 | Varian, Inc. | Method for determination of drugs of abuse in biological samples |
| CN1818635A (en) * | 2006-03-15 | 2006-08-16 | 首都师范大学 | THz inspection and fingerprint spectrum for 12 drugs |
| CN101750458A (en) * | 2009-11-05 | 2010-06-23 | 香港科技大学 | Method for detecting drug residues in human body |
| CN102128905A (en) * | 2010-12-10 | 2011-07-20 | 中国广州分析测试中心 | Method for quickly detecting drug |
Non-Patent Citations (1)
| Title |
|---|
| 张学成 等: "海洛因标准品的制备", 《刑事技术》, 30 June 1993 (1993-06-30), pages 25 - 27 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102759476A (en) * | 2012-07-20 | 2012-10-31 | 公安部禁毒情报技术中心 | Preparation method of cocaine hydrochloride standard substance |
| CN102749402A (en) * | 2012-08-07 | 2012-10-24 | 公安部禁毒情报技术中心 | Preparation method of morphine hydrochloride standard substance |
| CN107304213A (en) * | 2016-04-20 | 2017-10-31 | 中国医药工业有限公司 | A kind of opium poppy extract-treated method and apparatus |
| CN107304213B (en) * | 2016-04-20 | 2021-08-20 | 李显林 | Method and equipment for processing poppy extract |
| CN107345946A (en) * | 2017-05-08 | 2017-11-14 | 公安部物证鉴定中心 | Method for preparing purified for the methcathinone standard substance of forensic science illicit drugs inspection |
| CN107478733A (en) * | 2017-05-08 | 2017-12-15 | 公安部物证鉴定中心 | Method for preparing purified for the codeine standard substance of forensic science illicit drugs inspection |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102565260B (en) | 2014-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102565260B (en) | Method for preparing diacetylmorphine hydrochloride standard substance | |
| CN103713077B (en) | The method of alpha-aminobutyric acid content in high effective liquid chromatography for measuring red colouring agent for food, also used as a Chinese medicine | |
| CN102898566A (en) | Preparation method of metal organic framework molecularly imprinted polymer used for enriching trace amounts of Metolcarb | |
| CN111505161A (en) | Method for detecting enantiomer of protected amino acid | |
| CN102288687B (en) | Method for analyzing and detecting impurities in ornithine aspartate | |
| CN111812259A (en) | Method for detecting alanyl glutamine impurity in compound amino acid injection | |
| CN104280475A (en) | Method for detecting content of amino acid and glycyl glutamine in compound amino acid (15) dipeptide (2) injection | |
| CN102323233A (en) | Reagent and method for detecting homocysteine (HCY) | |
| CN105319309A (en) | Separation and detection method of glycyl-L-glutamine chiral isomer | |
| CN110849980A (en) | Method for detecting content of enantiomer in isopropyl L-alanine | |
| CN106117308A (en) | A kind of preparation method of Imidapril Hydrochloride | |
| CN104515820A (en) | Tigecycline intermediate analysis detection method | |
| CN108072717B (en) | Method for detecting arginine solution | |
| CN106018573B (en) | Hydrochloric acid replaces the method for detecting purity than drawing west in a kind of TAS-102 | |
| CN104961716A (en) | Method for separating high-purity lactone type lovastatin from fermentum rubrum powder | |
| CN102875326B (en) | A kind of azeotropic-absorption method prepares the method for high-pure anhydrous methyl alcohol | |
| CN107315055B (en) | Content determination method of agmatine sulfate | |
| CN103412082B (en) | HPLC (High Performance Liquid Chromatography) technique-based detection method for contents of jasmonic acid compounds in lycoris radiate | |
| CN105486788A (en) | Kit for determining zeatin nucleoside content and method thereof | |
| CN104483419A (en) | Detection method of bortezomib intermediate | |
| CN108872405A (en) | A kind of HPLC analyzing detecting method of the lodoxamide tromethamine in relation to substance | |
| CN101762665B (en) | Method for measuring tyrosine, phenylalanine and tryptophane in wort, fermentation liquid and beer | |
| CN111044636A (en) | Analytical method of micafungin content | |
| CN105717206A (en) | Method for separating and determining calcipotriol intermediate F and impurities thereof | |
| CN102491926B (en) | Method for preparing and purifying tiopronin disulphide |
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 |